CN115403786A - Humic acid shale inhibitor and preparation method and application thereof - Google Patents
Humic acid shale inhibitor and preparation method and application thereof Download PDFInfo
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- CN115403786A CN115403786A CN202110592795.XA CN202110592795A CN115403786A CN 115403786 A CN115403786 A CN 115403786A CN 202110592795 A CN202110592795 A CN 202110592795A CN 115403786 A CN115403786 A CN 115403786A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/04—Aqueous well-drilling compositions
- C09K8/14—Clay-containing compositions
- C09K8/18—Clay-containing compositions characterised by the organic compounds
- C09K8/22—Synthetic organic compounds
- C09K8/24—Polymers
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Abstract
The invention provides a preparation method of a humic acid shale inhibitor, which comprises the following steps: adding humic acid, sodium hydroxide and water under stirring, and reacting for 1 hour at 70 ℃ to obtain a mixture; adding polyamine A and formaldehyde into the mixture to react to obtain a reaction product; and adding polyamine B and epoxy chloropropane into the reaction product under the stirring state for reaction, drying and crushing the obtained reaction product at 70 ℃ to obtain the humic acid shale inhibitor. The modified humic acid shale inhibitor prepared by the invention is obtained by modifying natural materials, is solid, is convenient to transport, has the characteristics of environmental protection, no toxicity and easy degradation, has good shale inhibition capacity, has a certain viscosity reduction effect and low foaming rate, does not greatly influence shearing force and filtration loss, and has good compatibility with drilling fluid. The invention also provides a humic acid shale inhibitor and a drilling fluid.
Description
Technical Field
The invention belongs to the technical field of drilling fluids, and particularly relates to a humic acid shale inhibitor, and a preparation method and application thereof.
Background
With the continuous exploitation of unconventional oil and gas resources, deep wells, ultra-deep wells, marine wells and wells in complex sections, when a shale stratum is encountered in the drilling process, the hydration expansion and dispersion of shale cause a series of problems of instability of a well wall, bit balling, well bore purification and the like, the drilling difficulty is increased, and higher requirements are provided for a drilling fluid system, particularly a shale inhibitor. The common shale inhibitors mainly comprise polymers, inorganic salts, asphalts, polyamine and the like, and the shale inhibitors have some defects, such as poor environmental protection and high cost, and cause more negative effects on the drilling fluid when the dosage is higher, such as phenomena of adhesion, flocculation, foaming and the like. Therefore, the shale inhibitor which is low in cost, strong in environmental protection performance and free of negative effects on the drilling fluid is of great significance.
Disclosure of Invention
In view of this, the invention aims to provide a humic acid shale inhibitor, a preparation method and an application thereof.
The invention provides a preparation method of a humic acid shale inhibitor, which comprises the following steps:
carrying out a first reaction on humic acid, sodium hydroxide and water to obtain a first reaction product;
carrying out a second reaction on the first reaction product, polyamine A and formaldehyde to obtain a second reaction product;
carrying out a third reaction on the second reaction product, polyamine B and epoxy chloropropane to obtain a humic acid shale inhibitor;
the polyamine A is selected from one of ethylenediamine, propylenediamine, butylenediamine, diethylenetriamine and triethylenetetramine;
the polyamine B is selected from dimethylamine or diethylamine.
Preferably, the mass ratio of the humic acid to the sodium hydroxide to the water to the polyamine A to the formaldehyde to the polyamine B to the epichlorohydrin is (20-30): 2: (50-60): (5-8): (10-12): (10-15): (14 to 18).
Preferably, the temperature of the first reaction is 65 to 75 ℃.
Preferably, the temperature of the second reaction is 80 to 90 ℃.
Preferably, the temperature of the third reaction is 60 to 70 ℃.
Preferably, the first reaction is carried out under stirring; the third reaction is carried out under stirring.
Preferably, the third reaction further comprises, after completion:
and drying and crushing the obtained reaction product to obtain the humic acid shale inhibitor.
Preferably, the drying temperature is 65 to 75 ℃.
The invention provides a humic acid shale inhibitor prepared by the method in the scheme.
A drilling fluid, comprising: the humic acid shale inhibitor in the technical scheme.
The biomass raw material has the advantages of environmental protection, easy biodegradation, low price and the like, but can not be directly used and needs to be modified by means of chemistry, biology and the like. The humic acid is a biomass resource with wide source and low material cost, so the humic acid has good prospect for preparing the shale inhibitor by modifying the humic acid.
The humic acid shale inhibitor provided by the invention is obtained by taking humic acid as a main agent and carrying out chemical modification. The humic acid shale inhibitor provided by the invention not only has the environmental protection performance of no toxicity, greenness and easy biodegradation, but also has the characteristics of low use cost, strong shale inhibition capability and the like, and the product has the advantages of simple and convenient production process, mild reaction conditions and low production cost.
Compared with the prior art, the preparation method of the modified humic acid shale inhibitor is obtained by modifying natural materials, and has the characteristics of wide raw material sources, excellent environmental protection, good biodegradability and the like. The shale inhibitor obtained by modification of humic acid not only has good shale inhibition capability, but also has the characteristics of no viscosity increase, no bubbling, wider use dosage, certain viscosity reduction capability and the like in the use process. Compared with the common liquid shale inhibitor, the humic acid modified shale inhibitor provided by the invention is solid, has simple and convenient production process and convenient transportation, and particularly has low humic acid material cost, so that the product cost is greatly reduced.
The cationic degree of the humic acid shale inhibitor provided by the invention is 2-4.5 mmol/g, and the relative inhibition rate is 97-99.5%.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other examples, which may be modified or appreciated by those skilled in the art based on the description of the embodiments, are intended to be within the scope of the present invention. It should be understood that the embodiments of the present invention are only for illustrating the technical effects of the present invention, and are not intended to limit the scope of the present invention. In the examples, the methods used are conventional methods unless otherwise specified.
The invention provides a preparation method of a humic acid shale inhibitor, which comprises the following steps:
carrying out a first reaction on humic acid, sodium hydroxide and water to obtain a first reaction product;
carrying out a second reaction on the first reaction product, polyamine A and formaldehyde to obtain a second reaction product;
carrying out a third reaction on the second reaction product, polyamine B and epichlorohydrin to obtain a humic acid shale inhibitor;
the polyamine A is selected from one of ethylenediamine, propylenediamine, butylenediamine, diethylenetriamine and triethylenetetramine;
the polyamine B is selected from dimethylamine or diethylamine.
In the present invention, the first reaction is preferably carried out under stirring. In the present invention, the temperature of the first reaction is preferably 65 to 75 ℃, more preferably 68 to 72 ℃, and most preferably 70 ℃; the time of the first reaction is preferably 0.5 to 1.5 hours, more preferably 0.8 to 1.2 hours, and most preferably 1 hour.
In the present invention, the method of the second reaction preferably includes:
and adding polyamine A and formaldehyde into the first reaction product to carry out a second reaction to obtain a second reaction product.
In the present invention, the temperature of the second reaction is preferably 80 to 90 ℃, more preferably 82 to 88 ℃, more preferably 84 to 86 ℃, and most preferably 90 ℃; the time for the second reaction is preferably 2 to 4 hours, more preferably 2.5 to 3.5 hours, and most preferably 2.5 hours or 3 hours.
In the present invention, the method of the third reaction preferably includes:
and adding polyamine B and epoxy chloropropane into the second reaction product to carry out a third reaction, thereby obtaining the humic acid shale inhibitor.
In the present invention, the temperature of the third reaction is preferably 60 to 70 ℃, more preferably 63 to 67 ℃, and most preferably 60 ℃; the time of the third reaction is preferably 5 to 7 hours, more preferably 5.5 to 6.5 hours, and most preferably 6 hours or 7 hours.
In the present invention, the polyamine a is preferably ethylenediamine or diethylenetriamine, more preferably diethylenetriamine.
In the present invention, the polyamine B is preferably dimethylamine.
In the invention, the mass ratio of the humic acid, the sodium hydroxide, the water, the polyamine A, the formaldehyde, the polyamine B and the epichlorohydrin is preferably (20-30): 2: (50-60): (5-8): (10-12): (10-15): (14 to 18), more preferably (23 to 27): 2: (53-57): (6-7): 11: (11-14): (15-17), most preferably 20:2:50:6:11:10:16.
the invention provides a humic acid shale inhibitor prepared by the method of the technical scheme; the preferred cationicity of the humic acid shale inhibitor is 2-4.5 mmol/g; the relative inhibition ratio is preferably 97 to 99.5%.
The invention provides a drilling fluid, which comprises: the humic acid shale inhibitor in the technical scheme.
The invention has no special limitation on other components of the drilling fluid, and a person skilled in the art can select a drilling fluid with proper components according to actual needs and add the shale inhibitor in the technical scheme.
In the present invention, the drilling fluid preferably comprises:
bentonite slurry, sulfonated phenolic resin, sulfonated lignite, sulfonated asphalt, sodium carboxymethyl cellulose, low polyanionic cellulose, sodium hydroxide, a humic acid shale inhibitor and barite.
In the present invention, the bentonite slurry is preferably a pre-hydrated bentonite slurry. In the present invention, the method for preparing the pre-hydrated bentonite slurry preferably comprises:
mixing sodium carbonate, bentonite and water, sealing and maintaining to obtain the prehydrated bentonite slurry.
In the present invention, the sodium carbonate is preferably anhydrous sodium carbonate.
In the present invention, the ratio of the amount of water, sodium carbonate and bentonite is preferably (350 to 450) mL: (0.5 to 0.6) g: (12-20) g, more preferably (380-420) mL: (0.52-0.58) g: (14-18) g, most preferably 400mL:0.56g:16g.
In the present invention, the mixing is preferably performed under stirring; the stirring speed is preferably 10000-12000 r/min, more preferably 10500-11500 r/min, and most preferably 11000r/min; the mixing time is preferably 15 to 25min, more preferably 18 to 22min, most preferably 20min.
In the present invention, the closed curing is preferably performed at room temperature, which is preferably 20 to 30 ℃, more preferably 22 to 28 ℃, more preferably 24 to 26 ℃, and most preferably 25 ℃; the time for the sealing and curing is preferably 20 to 30 hours, more preferably 22 to 25 hours, and most preferably 24 hours.
In the present invention, the sulfonated phenolic resin is preferably a sulfonated phenolic resin type II (e.g., SMP-2); the mass volume ratio of the sulfonated phenolic resin in the bentonite slurry is preferably 2 to 6%, more preferably 3 to 5%, and most preferably 4%.
In the present invention, the mass-to-volume ratio of the sulfonated lignite (SMC) in the bentonite slurry is preferably 2 to 6%, more preferably 3 to 5%, and most preferably 4%.
In the present invention, the mass-to-volume ratio of the sulfonated asphalt (FT-1) in the bentonite slurry is preferably 2 to 4%, more preferably 2.5 to 3.5%, and most preferably 3%.
In the present invention, the mass-to-volume ratio of the carboxymethyl cellulose sodium salt (LV-CMC) in the bentonite slurry is preferably 0.1 to 0.3%, more preferably 0.15 to 0.25%, and most preferably 0.2%.
In the present invention, the mass-to-volume ratio of the low polyanionic cellulose (LV-PAC) in the bentonite slurry is preferably 0.5 to 0.9%, more preferably 0.6 to 0.8%, and most preferably 0.7%.
In the present invention, the mass-to-volume ratio of the sodium hydroxide in the bentonite slurry is preferably 0.3 to 0.7%, more preferably 0.4 to 0.6%, and most preferably 0.5%.
In the invention, the mass-to-volume ratio of the humic acid shale inhibitor in the bentonite slurry is preferably 0.5-1.5%, more preferably 0.8-1.2%, and most preferably 1%.
In the present invention, the amount of the barite is preferably such that the density of the drilling fluid is 1 to 2g/cm 3 More preferably 1.2 to 1.8g/cm 3 More preferably 1.4 to 1.6g/cm 3 Most preferably 1.5g/cm 3 。
In the present invention, the preparation method of the drilling fluid preferably comprises:
sequentially adding sulfonated phenolic resin, sulfonated lignite and sulfonated asphalt into the bentonite slurry to carry out first high-speed stirring; then adding sodium carboxymethyl cellulose and low polyanion cellulose to carry out second high-speed stirring; and then adding sodium hydroxide and a humic acid shale inhibitor for third high-speed stirring, and finally adding barite for fourth high-speed stirring to obtain the drilling fluid.
In the present invention, the time of the first high-speed stirring is preferably 3 to 7min, more preferably 4 to 6min, and most preferably 5min; the second high-speed stirring time is preferably 8-12 min, more preferably 9-11 min, and most preferably 10min; the third high-speed stirring time is preferably 3 to 7min, more preferably 4 to 6min, and most preferably 5min; the fourth high-speed stirring time is preferably 15 to 25min, more preferably 18 to 22min, and most preferably 20min.
In the present invention, the high-speed stirring speed is preferably 10000 to 11000r/min, more preferably 10200 to 10800r/min, more preferably 10400 to 10600r/min, and most preferably 10500r/min.
The modified humic acid shale inhibitor prepared by the method has the shale inhibitor capability equivalent to that of the traditional polyamine and polyether amine shale inhibitors, almost has no influence on the rheological property, the filtration loss and other properties of the drilling fluid, and has no viscosity increase, no foaming and wide use dosage. The modified humic acid shale inhibitor prepared by the invention has the advantages of mild and simple production process, wide raw material source, low cost, excellent environmental protection and biodegradability, and is convenient to transport and use, and the main agent of the inhibitor is humic acid.
Humic acid used in the following examples of the present invention was purchased from yunnan double-dragon brown source humic acid limited; sodium hydroxide, ethylenediamine, diethylenetriamine, dimethylamine, diethylamine and epichlorohydrin are all purchased from Aladdin reagents Co.Ltd; sulfonated phenol-formaldehyde resin type II (SMP-2) was purchased from Shandong Shunyuan Petroleum science and technology Co., ltd; sulfonated lignite (SMC) was purchased from Desheng drilling fluid science and technology works in Henan; sulfonated asphalt (FT-1) was purchased from seventh chemical Co., ltd, new county, henan province; bentonite, sodium carboxymethyl cellulose (LV-CMC) was purchased from Puyang central three industries, inc.; low polyanionic cellulose (LV-PAC) was purchased from Zheng Zhou Oriental Assistant Co., ltd.
The relative inhibition rate of the modified humic acid shale inhibitor prepared in the following embodiment of the invention is determined according to the standard Q/SH0323-2009 shale inhibitor technical requirement for drilling fluid, and the cationic degree is determined according to the method of the literature Yangtze river, application research of composite cationic polyamine shale inhibitor. LD in the embodiment of the invention 50 The values were measured according to the Standard "test methods for acute oral toxicity of Chemicals" (GB/T21603-2008) and "test methods for acute inhalation toxicity of Chemicals" (GB/T21605-2008), and BOD 5 /COD Cr The values were determined according to standard environmental protection requirements for water-soluble oilfield chemicals (SY/T6787-2010).
Example 1
Under a stirring state, 20 parts by mass of humic acid, 50 parts by mass of water and 2 parts by mass of sodium hydroxide are added into a reaction kettle, and the mixture is obtained after reaction for 1 hour at 70 ℃. Adding 6 parts by mass of diethylenetriamine and 11 parts by mass of formaldehyde into the mixture, reacting at 90 ℃ for 2.5 hours, adding 10 parts by mass of dimethylamine and 18 parts by mass of epichlorohydrin, reacting at 60 ℃ for 7 hours, drying and crushing the obtained reaction product at 70 ℃ to obtain the modified humic acid shale inhibitor.
Example 2
Under a stirring state, 20 parts by mass of humic acid, 50 parts by mass of water and 2 parts by mass of sodium hydroxide were added to a reaction kettle, and a reaction was carried out at 70 ℃ for 1 hour to obtain a mixture. Adding 8 parts by mass of ethylenediamine and 12 parts by mass of formaldehyde into the mixture, reacting at 80 ℃ for 4 hours, adding 15 parts by mass of dimethylamine and 16 parts by mass of epichlorohydrin, reacting at 70 ℃ for 6 hours, drying and crushing the obtained reaction product at 70 ℃ to obtain the modified humic acid shale inhibitor.
Example 3
Under a stirring state, 20 parts by mass of humic acid, 50 parts by mass of water and 2 parts by mass of sodium hydroxide are added into a reaction kettle, and the mixture is obtained after reaction for 1 hour at 70 ℃. Adding 6 parts by mass of diethylenetriamine and 11 parts by mass of formaldehyde into the mixture, reacting at 90 ℃ for 2.5h, adding 13 parts by mass of diethylamine and 14 parts by mass of epichlorohydrin, reacting at 60 ℃ for 5h, drying and crushing the obtained reaction product at 70 ℃ to obtain the modified humic acid shale inhibitor.
Example 4
Under a stirring state, 30 parts by mass of humic acid, 60 parts by mass of water and 2 parts by mass of sodium hydroxide are added into a reaction kettle, and the mixture is obtained after reaction for 1 hour at 70 ℃. Adding 8 parts by mass of diethylenetriamine and 12 parts by mass of formaldehyde into the mixture, reacting at 85 ℃ for 3 hours, adding 15 parts by mass of dimethylamine and 18 parts by mass of epichlorohydrin, reacting at 65 ℃ for 6 hours, drying and crushing the obtained reaction product at 70 ℃ to obtain the modified humic acid shale inhibitor.
Performance detection
The modified humic acid shale inhibitor prepared in the embodiments 1 to 4 of the invention is subjected to relative inhibition rate, cationic degree and LD 50 、BOD 5 /COD Cr The performance test results are shown in table 1.
Table 1 performance testing of modified humic acid shale inhibitors prepared in accordance with the present examples
As can be seen from Table 1, the modified humic acid shale inhibitors prepared in examples 1 to 4 have a relative inhibition rate of 95.0% to 99.5% and a cationic degree of 2.0 to 4.5mmol/L; shows that the modified humic acid shale inhibitor has excellent inhibition capability, higher cationic degree and LD 50 ＞5000mg/kg，BOD 5 /COD Cr More than 0.5, the modified humic acid shale inhibitor has the advantages of no toxicity, easy biodegradability and excellent environmental protection performance.
Example 5
Bentonite prehydration: adding 400mL of water into a stirring cup, adding 0.56g of anhydrous sodium carbonate and 16g of bentonite while stirring, stirring at a high speed of 11000r/min for 20min, and sealing and maintaining at room temperature for 24h to obtain prehydrated bentonite slurry.
Based on the total volume of the prehydrated bentonite slurry: sequentially adding SMP-2 with the mass volume ratio of 4%, SMC with the mass volume ratio of 4% and FT-1 with the mass volume ratio of 3% into the bentonite slurry, and stirring at a high speed for 5min; then adding 0.2% of LV-CMC and 0.7% of LV-PAC in mass volume ratio, and stirring at high speed for 10min; then adding 0.5 percent of sodium hydroxide by mass volume ratio, and stirring at high speed for 5min; finally adding barite to adjust the density of the drilling fluid to 1.5g/cm 3 And stirring at a high speed for 20min to obtain the drilling fluid.
Example 6
A drilling fluid was prepared according to the preparation method of example 5, which is different from example 5 in that 1% by mass by volume of the modified humic acid shale inhibitor prepared in example 1 was further added to the bentonite slurry.
Example 7
A drilling fluid was prepared according to the method of example 6, differing from example 6 in that the modified humic acid shale inhibitor prepared in example 2 was used instead of the modified humic acid shale inhibitor prepared in example 1.
Example 8
A drilling fluid was prepared according to the method of example 6, differing from example 6 in that the modified humic acid shale inhibitor prepared in example 3 was used instead of the modified humic acid shale inhibitor prepared in example 1.
Example 9
A drilling fluid was prepared according to the method of example 6, differing from example 6 in that the modified humic acid shale inhibitor prepared in example 4 was used instead of the modified humic acid shale inhibitor prepared in example 1.
Example 10
A drilling fluid was prepared according to the method of example 6, differing from example 6 in that a mass to volume ratio of 4% was used instead of 1% in example 6.
Performance detection
The drilling fluid prepared in the embodiments 5-10 of the invention is put into an aging kettle, placed in a roller furnace, rolled for 16h at 150 ℃, and then the performance of the drilling fluid is determined, wherein the performance determination method is according to the national standard GB/T16783.1-2014, part 1 of the field test of the drilling fluid in the petroleum and gas industry: the water-based drilling fluid is detected, the detection result is shown in table 2, and table 2 shows the performance test result of the drilling fluid prepared in the embodiment of the invention.
Table 2 drilling fluid performance test results prepared in the examples of the present invention
In Table 2, AV is the apparent viscosity, PV is the plastic viscosity, YP is the dynamic shear force, Q 10s /Q 10min For initial and final cut, FL is the API filtrate loss.
As can be seen from table 2, the modified humic acid shale inhibitor prepared in the examples of the present invention has a certain viscosity reduction effect, but has little influence on shearing force and fluid loss, and after the shale inhibitor is added, the drilling fluid hardly foams, and even if the addition amount is 4%, the foaming rate is less than 5%. Therefore, the modified humic acid shale inhibitor prepared by the invention has little influence on the drilling fluid and good compatibility.
The modified humic acid shale inhibitor prepared by the method has the shale inhibitor capability equivalent to that of the traditional polyamine and polyether amine shale inhibitors, almost has no influence on the rheological property, the filtration loss and other properties of the drilling fluid, and has no viscosity increase, no foaming and wide use dosage. The modified humic acid shale inhibitor prepared by the invention has the advantages of mild and simple production process, wide raw material source, low cost, excellent environmental protection and biodegradability, and the main agent is humic acid, and the product is solid and is convenient to transport and use.
While only the preferred embodiments of the present invention have been described, it should be understood that various modifications and adaptations thereof may occur to one skilled in the art without departing from the spirit of the present invention and should be considered as within the scope of the present invention.
Claims (10)
1. A preparation method of a humic acid shale inhibitor comprises the following steps:
carrying out a first reaction on humic acid, sodium hydroxide and water to obtain a first reaction product;
carrying out a second reaction on the first reaction product, polyamine A and formaldehyde to obtain a second reaction product;
carrying out a third reaction on the second reaction product, polyamine B and epoxy chloropropane to obtain a humic acid shale inhibitor;
the polyamine A is selected from one of ethylenediamine, propylenediamine, butylenediamine, diethylenetriamine and triethylenetetramine;
the polyamine B is selected from dimethylamine or diethylamine.
2. The method according to claim 1, wherein the mass ratio of the humic acid to the sodium hydroxide to the water to the polyamine A to the formaldehyde to the polyamine B to the epichlorohydrin is (20-30): 2: (50-60): (5-8): (10-12): (10-15): (14 to 18).
3. The method of claim 1, wherein the temperature of the first reaction is 65 to 75 ℃.
4. The method of claim 1, wherein the temperature of the second reaction is 80 to 90 ℃.
5. The method of claim 1, wherein the temperature of the third reaction is 60 to 70 ℃.
6. The process according to claim 1, characterized in that the first reaction is carried out under stirring conditions; the third reaction is carried out under stirring.
7. The method of claim 1, further comprising, after the third reaction is completed:
and drying and crushing the obtained reaction product to obtain the humic acid shale inhibitor.
8. The method according to claim 7, wherein the temperature of the drying is 65 to 75 ℃.
9. A humic acid shale inhibitor prepared by the method of claim 1.
10. A drilling fluid, comprising: the humic acid shale inhibitor of claim 9.
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