CN113698510A - Modified chitosan as environment-friendly bionic shale inhibitor for water-based drilling fluid - Google Patents
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Abstract
The invention relates to the field of oilfield chemistry in the petroleum industry, in particular to an environment-friendly bionic shale inhibitor for water-based drilling fluid, which is prepared from modified chitosan. The invention provides application of modified chitosan serving as a shale inhibitor in drilling fluid, wherein a modified group with a structure shown in a formula (1) is connected to the modified chitosan; formula (1): -CH2‑CH(OH)CH2-a polyamine structure; the polyamine structure is provided by polyamine compounds. The modified chitosan provided by the invention can be used as a shale inhibitor to effectively inhibit hydration expansion and dispersion of shale, has no negative effect on the performance of drilling fluid, has no toxic or side effect, and can improve the stability of the well wall of a shale oil-gas well.
Description
Technical Field
The invention relates to the field of oilfield chemistry in the petroleum industry, in particular to an environment-friendly bionic shale inhibitor for water-based drilling fluid, which is prepared from modified chitosan.
Background
With the continuous increase of global oil and gas resource demand and the gradual depletion of conventional oil and gas resources, the exploration and development of unconventional oil and gas resources are greatly valued by various large oil and gas operators at home and abroad, particularly shale oil and gas resources. However, the shale stratum stored drilling well is easy to generate borehole wall instability, and the shale oil gas is seriously hindered from being safely and efficiently explored and developed. One type of shale is a rock mineral rich in various clays which are easy to hydrate, and when the water-based drilling fluid is used for drilling a shale stratum, the shale is easy to hydrate, expand and disperse, so that the borehole wall is unstable, and the drilling cost is greatly increased. Therefore, inhibition of shale hydration becomes one of the key technologies which need to be solved urgently in the shale oil and gas exploration and development process. The oil-based drilling fluid is considered to be the most effective system for avoiding hydration expansion and dispersion of shale formation, but has the problems of high cost, environmental pollution, influence on well cementation quality and the like. Therefore, various shale inhibitors suitable for water-based drilling fluids have been developed at home and abroad to keep the borehole wall stable. At present, the most widely used shale inhibitor is KCl, however, the high concentration of KCl can seriously harm the ecosystem, so various environment-friendly amine-based inhibitors such as polyamino acid, polyether amine, small cation quaternary ammonium salt and the like are developed. Despite the advances made, there are still some disadvantages. The amino-terminated polymers have low content of terminal amino groups, so that the inhibition capability is limited, and when the addition amount is too large, the drilling fluid loss is increased, so that the drilling stability is deteriorated, and the requirement of shale oil and gas drilling cannot be met. Therefore, further development of environmentally friendly high performance amine-based shale inhibitors is necessary.
Disclosure of Invention
The invention aims to overcome the problem that the existing inhibitor is not ideal in performance, meet the environmental protection target and develop an environment-friendly bionic shale inhibitor capable of effectively inhibiting hydration expansion of mud shale, and in order to achieve the aim, on one hand, the invention provides application of modified chitosan as a shale inhibitor in drilling fluid, wherein the modified chitosan is connected with a modified group with a structure shown in a formula (1);
formula (1): -CH2-CH(OH)CH2-a polyamine structure; said pluralityThe amine structure is provided by polyamine compounds.
The invention provides a water-based drilling fluid containing modified chitosan as a shale inhibitor, wherein a modifying group with a structure shown in a formula (1) is connected to the modified chitosan;
formula (1): -CH2-CH(OH)CH2-a polyamine structure; the polyamine structure is provided by polyamine compounds.
In a third aspect the invention provides the use of the above water-based drilling fluid in oil and gas drilling.
The modified chitosan provided by the invention can effectively inhibit hydration expansion and dispersion of shale as a shale inhibitor, can improve the stability of the well wall of a shale oil-gas well, has no negative effect on the performance of drilling fluid, is nontoxic, and has important practical value and economic benefit for further promoting the exploration and development of shale oil-gas resources in China.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides an application of modified chitosan as a shale inhibitor in drilling fluid, wherein a modified group with a structure shown in a formula (1) is connected to the modified chitosan;
formula (1): -CH2-CH(OH)CH2-a polyamine structure; the polyamine structure is provided by polyamine compounds.
Preferably, the molecular weight of the chitosan is 20000-100000g/mol, preferably 40000-90000g/mol, more preferably 50000-85000g/mol, such as 50000-75000 g/mol.
Preferably, the polyamine structure may be, for example, -NH- (CH)2CH2NH)n-CH2CH2-NH2Or is orThese are-NH-polyamine residues.
Preferably, the polyamine compound is one or more of polyene polyamine and polyethyleneimine, preferably one or more of diethylenetriamine, triethylene tetramine, tetraethylene pentamine and polyethyleneimine. The polyethyleneimine may be, for example, polyethyleneimine having a molecular weight of 300-5000g/mol (preferably 600-3000g/mol, more preferably 600-1500 g/mol).
Preferably, the modification group with the structure shown in the formula (1) is provided by reacting epichlorohydrin and a polyamine compound.
Preferably, the content of the modifying group having a structure represented by the formula (1) is 5 to 25% by weight, preferably 8 to 20% by weight, more preferably 8.5 to 17% by weight, relative to the total amount of the modified chitosan.
Preferably, the chitosan is connected with the modified group of the structure shown in the formula (1) through a group provided by benzaldehyde.
The invention also provides an application of the modified chitosan as a shale inhibitor in drilling fluid, wherein the preparation method of the modified chitosan comprises the following steps:
(1) carrying out acidification swelling treatment on chitosan;
(2) in an alcohol solvent, carrying out a first contact reaction on acidified and swollen chitosan and benzaldehyde;
(3) in a first alkaline solution, carrying out a second contact reaction on the product obtained after the first contact reaction and epichlorohydrin;
(4) and (3) in a second alkaline solution, carrying out a third contact reaction on the product of the second contact reaction and the polyamine compound so as to enable the chitosan to be connected with the modified group with the structure shown in the formula (1).
According to the present invention, the swelling treatment may be a chitosan swelling treatment process which is conventional in the art, for example, chitosan may be contacted with an acidic solution to induce swelling of chitosan, which may be an aqueous glacial acetic acid solution, an aqueous hydrochloric acid solution, etc., and may have a concentration of, for example, 1 to 5 wt%, and may be used in an amount ranging from 10 to 30mL, relative to 1g of chitosan. The conditions for the swelling treatment may be, for example: the temperature is 20-40 deg.C, and the time is 20-60 min.
After the swelling treatment, the first contact reaction can be directly carried out under the condition of introducing an alcohol solvent and benzaldehyde. Preferably, the conditions of the first contact reaction include: the temperature is 60-80 ℃ and the time is 5-8 h. Wherein, the reaction of benzaldehyde and chitosan is the condensation reaction of benzoic acid and chitosan which is conventional in the field. After the first contact reaction, the reaction product may be washed and dried.
The alcohol solvent may be an alcohol or an alcohol-water mixture, preferably an alcohol, wherein the alcohol may be one or more of methanol, ethanol, n-propanol, etc., and may be used in a wide range, for example, in an amount of 10 to 100mL, for example, 20 to 50mL, relative to 1g of chitosan.
According to the invention, the product obtained by the first contact reaction is subjected to a second contact reaction with epichlorohydrin in a first alkaline solution, so that a group with a propylene oxide structure can be substituted on chitosan, and a subsequent third contact reaction is carried out to react with an amine group. Wherein, preferably, the conditions of the second contact reaction comprise: the temperature is 45-60 ℃ and the time is 3-6 h.
According to the invention, the first alkaline solution may be an aqueous solution of an alkaline agent, for example one or more selected from sodium hydroxide, potassium hydroxide, lithium hydroxide, etc., in a concentration of, for example, 0.2 to 0.6mol/L, or ammonia, in a wide range, for example 50 to 200mL, relative to 1g of chitosan.
After the second contact reaction, washing and drying the reaction product.
According to the invention, the product obtained by the second contact reaction is subjected to a third contact reaction with a polyamine compound in a second alkaline solution, so that a modified group comprising a polyamine group can be formed on the chitosan. Wherein, preferably, the conditions of the third contact reaction comprise: the temperature is 50-80 ℃ and the time is 3-6 h.
According to the invention, the second alkaline solution may be an aqueous solution of an alkaline agent, for example one or more selected from sodium hydroxide, potassium hydroxide, lithium hydroxide, etc., in a concentration of, for example, 0.02-0.3mol/L, or in an amount varying within wide limits, for example, 50-200mL of the first alkaline solution with respect to 1g of chitosan, or ammonia.
Preferably, the weight ratio of the dosage of the chitosan to the dosage of the benzaldehyde is 1:2-6, preferably 1: 2-4;
preferably, the weight ratio of the chitosan to the epichlorohydrin is 1:5-20, preferably 1: 8-15;
preferably, the weight ratio of the epoxy chloropropane to the polyamine compound is 1: 0.05-0.5.
The third aspect of the invention provides a water-based drilling fluid containing modified chitosan as a shale inhibitor, wherein a modifying group with a structure shown in a formula (1) is connected to the modified chitosan;
formula (1): -CH2-CH(OH)CH2-a polyamine structure; the polyamine structure is provided by polyamine compounds.
The modified chitosan is as described above, and the present invention is not described herein again.
In a fourth aspect, the invention provides the use of the above-described water-based drilling fluid in oil and gas drilling.
The modified chitosan provided by the invention as an environment-friendly bionic shale inhibitor has the following advantages: the drilling fluid still has good inhibition performance on the premise of not influencing the stability of the drilling fluid; the material has good temperature resistance, and can resist the temperature of more than 220 ℃; no biological toxicity and biodegradability, thus being environment-friendly; not only can inhibit osmotic hydration, but also can inhibit the occurrence of surface hydration; the shale rock debris dispersion can be effectively inhibited, the rock hydration and expansion of the well wall are prevented, the mud-coated drill bit is prevented, and finally the purposes of stabilizing the well wall and improving the mechanical drilling speed are achieved.
The present invention will be described in detail below by way of examples.
Environment-friendly bionic shale inhibitor example 1
The following examples are provided to illustrate the environmentally friendly biomimetic shale inhibitors and methods of making the same according to the present invention.
(1) 3g of chitosan (molecular weight 50000g/mol) was weighed into 40ml of 2 wt% glacial acetic acid aqueous solution and swelled for 30 min.
(2) Then diluting with 40mL of absolute ethyl alcohol, adjusting the pH value to 5, dropwise adding 11.7g of benzaldehyde, heating in a water bath to 70 ℃, stirring for reacting for 6 hours, cooling to room temperature, washing with ethanol and diethyl ether, and drying at constant temperature to obtain a solid product A.
(3) And heating the product solid A and 250ml of 0.4mol/L NaOH aqueous solution in a water bath to 55 ℃, adding 30ml of epoxy chloropropane, stirring and reacting for 5 hours, cooling to room temperature, washing with acetone and diethyl ether for 2 times respectively, and drying in vacuum at 60 ℃ to obtain a solid product B.
(4) And finally heating the solid product B and 180ml of 0.1mol/L NaOH aqueous solution in a water bath to 60 ℃, adding 13g of polyethyleneimine (with the molecular weight of 1000g/mol), stirring for reaction for 4 hours, cooling to room temperature, precipitating the product with acetone, drying and crushing to obtain a powdery reaction product, namely the environment-friendly bionic shale inhibitor EFYZ-1, wherein the content of a modified group provided by epichlorohydrin and the polyethyleneimine is 14.5 wt%.
Environment-friendly bionic shale inhibitor example 2
The following examples are provided to illustrate the environmentally friendly biomimetic shale inhibitors and methods of making the same according to the present invention.
(1) 3g of chitosan (molecular weight 75000g/mol) was weighed out and added to 40ml of 2% glacial acetic acid to swell for 30 min.
(2) Then diluting with 50mL of absolute ethyl alcohol, adjusting the pH value to 5, dropwise adding 10g of benzaldehyde, heating in a water bath to 65 ℃, stirring for reaction for 7 hours, cooling to room temperature, washing with ethanol and diethyl ether, and drying at constant temperature to obtain a solid product A.
(3) And then heating the product solid A and 250ml of 0.5mol/L NaOH aqueous solution in a water bath to 60 ℃, adding 25ml of epoxy chloropropane, stirring and reacting for 5 hours, cooling to room temperature, washing for 2 times respectively by using acetone and diethyl ether, and drying in vacuum at 60 ℃ to obtain a solid product B.
(4) And finally heating the solid product B and 180ml of 0.0.5mol/LNaOH aqueous solution in a water bath to 70 ℃, adding 10g of polyethyleneimine (with the molecular weight of 600g/mol), stirring for reacting for 4 hours, cooling to room temperature, precipitating the product with acetone, drying and crushing to obtain a powdery reaction product, namely the environment-friendly bionic shale inhibitor EFYZ-2, wherein the content of a modified group provided by epichlorohydrin and polyethyleneimine is 9.0 wt%.
Examples 3 to 5 of Environment-friendly Bionically-formed shale inhibitor
The following examples are provided to illustrate the environmentally friendly biomimetic shale inhibitors and methods of making the same according to the present invention.
The method of embodiment 1, except that:
example 3: in the step (4), 6g of diethylenetriamine is adopted to replace polyethyleneimine, and the environment-friendly bionic shale inhibitor EFYZ-3 is prepared through the whole reaction process;
example 4: 6g of triethylene tetramine is adopted to replace polyethyleneimine in the step (4), and the environment-friendly bionic shale inhibitor EFYZ-4 is prepared through the whole reaction process;
example 5: and (4) replacing polyethyleneimine with 6g of tetraethylenepentamine, and preparing the environment-friendly bionic shale inhibitor EFYZ-5 through the whole reaction process.
Suppression Performance test example 1
(1) Rolling recovery rate of shale: taking 20g of 6-10 meshes of shale debris, respectively placing the shale debris in 2% of KCl, 2% of polyetheramine and 2% of an environment-friendly bionic shale inhibitor aqueous solution, hot rolling for 16h at 150 ℃, sieving with a 40-mesh sieve for recovery, drying, weighing, and calculating the rolling recovery rate.
(2) Linear expansion ratio: weighing 5g of sodium bentonite in a core sleeve, pressing and holding the core sleeve for 5min under 10MPa, adding 2% of KCl, 2% of polyetheramine and 2% of an environment-friendly bionic shale inhibitor aqueous solution into a test sleeve, and performing an expansibility experiment by adopting a normal-temperature normal-pressure CPZ-II two-channel shale expansion instrument (Qingdao Jiaonan analyzer factory).
The test results are shown in the following table.
TABLE 1
The table shows that the environment-friendly bionic shale inhibitor has good inhibition performance, can obviously improve the rolling recovery rate of the shale in water, and reduces the linear expansion rate of the sodium bentonite.
Drilling fluid rheology and fluid loss performance test example 2
The environment-friendly bionic shale inhibitor with different concentrations is added into base slurry (the base slurry comprises 2 wt% of bentonite, 0.1 wt% of sodium carbonate, 0.02 wt% of sodium hydroxide and the balance of water), the rheological property of the base slurry is measured by a six-speed viscometer, the test result is shown in the following table, and the test method is as follows:
"PV" refers to the plastic viscosity in mPa · s measured by a van-type six-speed viscometer;
PV＝θ600-θ300
"AV" means the apparent viscosity, as measured by a van-type six-speed viscometer, in mPa · s units;
"YP" means dynamic shear force, calculated from data measured with a normal six-speed viscometer, in Pa;
YP＝0.511(θ300-PV)
“φ6/φ3"is the viscosity of the drilling fluid at low shear rate measured by a van-type six-speed viscometer without dimension;
“FLAPI"refers to the medium pressure fluid loss, measured by a medium pressure fluid loss gauge, in mL.
TABLE 2
As can be seen from the data results in Table 2, the environment-friendly bionic shale inhibitor has little influence on the rheological property and the fluid loss property of the base slurry, and has no obvious phenomena of viscosity increasing/reducing, and fluid loss increasing/fluid loss reducing. With the increase of the addition of the environment-friendly bionic shale inhibitor, the viscosity and the shearing force of the drilling fluid are not increased, and the drilling fluid has a slight dilution effect, so that the flow pattern of the drilling fluid is more favorably adjusted.
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, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. The application of the modified chitosan serving as a shale inhibitor in drilling fluid is characterized in that a modifying group with a structure shown in a formula (1) is connected to the modified chitosan;
formula (1): -CH2-CH(OH)CH2-a polyamine structure; the polyamine structure is provided by polyamine compounds.
2. The use according to claim 1, wherein the polyamine-based compound is one or more of a polyene polyamine and a polyethyleneimine, preferably one or more of diethylenetriamine, triethylenetetramine, tetraethylenepentamine and a polyethyleneimine;
preferably, the modification group with the structure shown in the formula (1) is provided by reacting epichlorohydrin with a polyamine compound;
preferably, the content of the modifying group is 5 to 25 wt%, preferably 8 to 20 wt%, more preferably 8.5 to 17 wt%, with respect to the total amount of the modified chitosan;
preferably, the chitosan is connected with the modified group of the structure shown in the formula (1) through a group provided by benzaldehyde.
3. The application of the modified chitosan serving as a shale inhibitor in drilling fluid is characterized in that the preparation method of the modified chitosan comprises the following steps:
(1) carrying out acidification swelling treatment on chitosan;
(2) in an alcohol solvent, carrying out a first contact reaction on acidified and swollen chitosan and benzaldehyde;
(3) in a first alkaline solution, carrying out a second contact reaction on the product obtained after the first contact reaction and epichlorohydrin;
(4) and in a second alkaline solution, performing a third contact reaction on the product of the second contact reaction and the polyamine compound to enable the chitosan to be connected with a modifying group.
4. The use of claim 3, wherein the conditions of the first contact reaction comprise: the temperature is 60-80 ℃, and the time is 5-8 h;
the conditions of the second contact reaction include: the temperature is 45-60 ℃, and the time is 3-6 h;
the conditions of the third contact reaction include: the temperature is 50-80 ℃ and the time is 3-6 h.
5. Use according to claim 3 or 4, wherein the chitosan and benzaldehyde are used in a weight ratio of 1:2-6, preferably 1: 2-4;
preferably, the weight ratio of the chitosan to the epichlorohydrin is 1:5-20, preferably 1: 8-15;
preferably, the weight ratio of the usage amount of the epichlorohydrin to the polyamine compound is 1: 0.05-0.5;
preferably, the molecular weight of the chitosan is 20000-100000g/mol, preferably 40000-90000g/mol, more preferably 50000-85000 g/mol.
6. A water-based drilling fluid containing modified chitosan as a shale inhibitor is disclosed, wherein a modifying group with a structure shown in a formula (1) is connected to the modified chitosan;
formula (1): -CH2-CH(OH)CH2-a polyamine structure; the polyamine structure is provided by polyamine compounds.
7. The water-based drilling fluid of claim 6, wherein the polyamine-based compound is one or more of a polyene polyamine and a polyethyleneimine, preferably one or more of diethylenetriamine, triethylenetetramine, tetraethylenepentamine and a polyethyleneimine;
preferably, the modification group with the structure shown in the formula (1) is provided by reacting epichlorohydrin with a polyamine compound;
preferably, the content of the modifying group is 5 to 25% by weight, preferably 8 to 20% by weight, more preferably 8.5 to 17% by weight, relative to the total amount of the modified chitosan.
8. The water-based drilling fluid of claim 6 or 7, wherein the modified chitosan is prepared by a method comprising:
(1) carrying out acidification swelling treatment on chitosan;
(2) in an alcohol solvent, carrying out a first contact reaction on acidified and swollen chitosan and benzaldehyde;
(3) in a first alkaline solution, carrying out a second contact reaction on the product obtained after the first contact reaction and epichlorohydrin;
(4) and (3) in a second alkaline solution, carrying out a third contact reaction on the product of the second contact reaction and the polyamine compound so as to enable the chitosan to be connected with the modified group with the structure shown in the formula (1).
9. The water-based drilling fluid of claim 8, wherein the conditions of the first contact reaction comprise: the temperature is 60-80 ℃, and the time is 5-8 h;
the conditions of the second contact reaction include: the temperature is 45-60 ℃, and the time is 3-6 h;
the conditions of the third contact reaction include: the temperature is 50-80 ℃ and the time is 3-6 h.
10. Use of the water-based drilling fluid according to any one of claims 6 to 9 in oil and gas drilling.
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| CN114350332A (en) * | 2020-08-26 | 2022-04-15 | 中国石油大学(北京) | Bionic and amphiphobic high-efficiency water-based drilling fluid |
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