CN114349958A - Synthesis of hyperbranched polylysine tertiary amine intercalation inhibitor and water-based drilling fluid - Google Patents
Synthesis of hyperbranched polylysine tertiary amine intercalation inhibitor and water-based drilling fluid Download PDFInfo
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- 238000009830 intercalation Methods 0.000 title claims abstract description 33
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- DTERQYGMUDWYAZ-ZETCQYMHSA-N N(6)-acetyl-L-lysine Chemical compound CC(=O)NCCCC[C@H]([NH3+])C([O-])=O DTERQYGMUDWYAZ-ZETCQYMHSA-N 0.000 claims description 12
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- JWCDUUFOAZFFMX-UHFFFAOYSA-N 2-ethenoxy-n,n-dimethylethanamine Chemical group CN(C)CCOC=C JWCDUUFOAZFFMX-UHFFFAOYSA-N 0.000 claims description 2
- KLPJXDPPMSJWKI-LURJTMIESA-N N(6)-formyl-L-lysine Chemical compound OC(=O)[C@@H](N)CCCCNC=O KLPJXDPPMSJWKI-LURJTMIESA-N 0.000 claims description 2
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Abstract
The invention discloses a synthesis method of a hyperbranched polylysine tertiary amine intercalation inhibitor and a water-based drilling fluid. The hyperbranched polylysine tertiary amine intercalation inhibitor is prepared by mixing hyperbranched polylysine tertiary amine and water, wherein the mass ratio of the hyperbranched polylysine tertiary amine in the drilling fluid is 0.5-5%. The hyperbranched polylysine tertiary amine synthesis raw material comprises ester substances containing polyene bonds, lysine substances containing secondary amine and alcohol substances with low molecular weight, and the end capping reagent is 1-methyl-2-propylene-1-amino methanol or 1-ethyl-2-propylene-1-amino methanol. The drilling fluid comprises the hyperbranched polylysine tertiary amine. The drilling fluid can effectively inhibit hydration expansion of shale. The shale intercalation inhibitor prepared from the hyperbranched polylysine tertiary amine provided by the invention is non-toxic and harmless, and the inhibition performance is obviously improved compared with the performance of similar intercalation inhibitors.
Description
Technical Field
The invention relates to the technical field of oil and gas field drilling, in particular to synthesis of a hyperbranched polylysine tertiary amine intercalation inhibitor and water-based drilling fluid containing the inhibitor.
Background
Borehole wall instability is one of the problems which seriously affect the drilling and production efficiency of oil and gas, and the direct or indirect economic loss caused by the accidents of diameter reduction, diameter expansion, drilling sticking and well collapse caused by the borehole wall instability reaches billions of dollars every year. Currently 75% of the formations being drilled or drilled belong to shale formations, and 90% of these borehole instability problems occur in shale formations. The reason is that the shale has strong water sensitivity, and when a shale stratum meets water, the shale stratum can generate serious hydration action, so that the shale generates phenomena of hydration expansion, dispersion and the like, and the stability of the well wall is reduced. In order to inhibit the hydration expansion of shale and improve the inhibition capability of water-based drilling fluid, the development of novel shale inhibitors is trending.
The polyamine high-performance drilling fluid system is a novel environment-friendly drilling fluid which meets the requirements of various aspects of the drilling process and is considered to replace oil-based drilling fluid, and domestic and international researches show that the polyamine inhibitor taking an amine monomer as a main raw material is widely applied to a water-based drilling fluid system and obtains a better inhibition effect, but the currently researched and applied polyamine inhibitor is mostly of a linear structure and is not uniformly wound and coated on clay, while a hyperbranched polymer has good solubility, excellent high rheological property and low viscosity property, on the other hand, the linear structure is easy to cause repeated adsorption or no adsorption, and action groups generally exist at two ends of a molecular chain, so that one molecular chain usually only contains two action groups, and the hyperbranched polymer has a series of unique physicochemical characteristics such as a large number of modifiable terminal functional groups and the like, therefore, the hyperbranched polyamine inhibitor has higher reactivity, and the research on the hyperbranched polyamine inhibitor is more needed.
Disclosure of Invention
Aiming at the problem of borehole wall instability caused by the fact that the conventional inhibitor cannot effectively inhibit the hydration expansion of shale at present, the invention provides a synthesis method of a hyperbranched polylysine tertiary amine intercalation inhibitor, which can effectively inhibit the hydration expansion problem of a shale stratum, thereby achieving the purpose of stabilizing the borehole wall.
In order to achieve the purpose, the technical scheme of the invention is as follows: a hyperbranched polylysine tertiary amine intercalation inhibitor and a water-based drilling fluid. The hyperbranched polylysine tertiary amine intercalation inhibitor comprises raw materials of ester substances containing polyene bonds and lysine substances containing secondary amine, wherein a blocking reagent is B-dimethylaminoethyl vinyl ether or 3- (ethyleneoxy) -N, N-dimethyl-1-propylamine, and the preparation steps are as follows:
(1) dissolving 0.5mol of lysine substances containing secondary amine in 100ml of methanol solution at normal temperature, then placing the lysine substance solution containing secondary amine in a closed container, performing reflux reaction for 12-14h under the condition of surrounding and stirring of nitrogen atmosphere, and then distilling the reaction product under reduced pressure to obtain lysine ester;
(2) respectively dissolving 0.3mol of lysine ester and 0.3mol of ester substance containing polyene bond in 100ml of organic solvent, dropwise adding the ester substance solution containing polyene bond into the lysine ester solution at 15-30 ℃ under the condition of nitrogen atmosphere and stirring, heating to 65-75 ℃ after dropwise adding, carrying out reflux reaction for 8-10h, and carrying out reduced pressure distillation to obtain hyperbranched polylysine;
(3) dissolving 0.2mol of hyperbranched polylysine in 100ml of organic solvent, dissolving 0.2mol of end-capping reagent in 50ml of organic solvent, dropwise adding the mixture into the hyperbranched polylysine solution under the condition of nitrogen atmosphere and stirring, heating to 65-70 ℃ after the titration is finished, carrying out closed reaction for 3 hours, and carrying out reduced pressure distillation after the reaction is finished to obtain a viscous product, namely the hyperbranched polylysine tertiary amine.
Further, the lysine-based substance containing the secondary amine in the step (1) is one of N6-acetyl-L-lysine and N epsilon-formyl-L-lysine.
Further, the ester substance containing the polyene bond is one of bis (vinylsulfonyl methyl) ether and bis (vinylsulfonyl) propanol.
Further, the organic solvent in the steps (2) and (3) is one of absolute methanol and absolute ethanol.
Further, the end-capping reagent is one of 1-methyl-2-propylene-1-amino methanol and 1-ethyl-2-propylene-1-amino methanol.
Further, the dripping time in the step (2) is controlled to be 35-45min, and the dripping time in the step (3) is controlled to be 40-50 min.
Further, the reduced pressure distillation temperature of the steps (1), (2) and (3) is 80-100 ℃, and the absolute vacuum degree is less than 3000 Pa.
The invention also aims to provide a water-based drilling fluid, which is added with the hyperbranched polylysine tertiary amine intercalation inhibitor.
The drilling fluid comprises the following components in parts by weight: based on 100 parts by weight of water, 2-4 parts by weight of bentonite and 0.3-0.4 part by weight of anhydrous Na2CO30.1-0.3 part of NaOH, 0.01-0.03 part of coating agent (KPAM), 0.3-0.8 part of salt-resistant agent (PAC-LV), 5-6 parts of filtrate reducer (SMP-1), 3-5 parts of anti-collapse agent (FRH), 4-5 parts of anti-seize lubricant (FK-10), 0.3-0.5 part of alkalinity regulator (CaO), 1-2 parts of shear strength agent (NH-1), 0.5-5 parts of inhibitor (hyperbranched polylysine tertiary amine intercalation inhibitor), 0-200 parts of weighting agent (nano-barite) (density is adjustable).
The invention has the following beneficial effects:
1. the product designed by the invention creatively responds to the requirement of environmental protection, has the advantages of biological non-toxicity, safety and easy degradation, and belongs to an environment-friendly inhibitor;
2. the synthesis method has stable and reliable technology, high yield and low price of raw materials required by the synthesized product, and is suitable for industrial production;
3. the shale inhibitor provided by the invention is hyperbranched polylysine tertiary amine, can effectively inhibit hydration expansion of a shale stratum, so that the effect of stabilizing a well wall is achieved, the inhibition performance is obviously improved compared with similar products, and the drilling requirements of various complex well conditions can be met.
Drawings
FIG. 1 is a molecular weight distribution diagram of hyperbranched polylysine tertiary amine S1 obtained in example 1;
FIG. 2 is a graph showing the molecular weight distribution of the hyperbranched polylysine tertiary amine S2 obtained in example 2.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the present examples, the parts are all parts by weight unless otherwise specified.
Firstly, synthesis of hyperbranched polylysine tertiary amine:
example 1:
preparing hyperbranched polylysine tertiary amine, namely dissolving 0.5mol of N6-acetyl-L-lysine in 100ml of methanol at normal temperature, then placing the N6-acetyl-L-lysine solution in a closed container, performing reflux reaction for 12h under the condition of surrounding and stirring of nitrogen atmosphere, and then performing reduced pressure distillation on a reaction product to obtain N6-acetyl-L-lysine methyl ester; respectively dissolving 0.3mol of N6-acetyl-L-lysine methyl ester and 0.3mol of bis (vinylsulfonylmethyl) ether in 100ml of organic solvent, dropwise adding a bis (vinylsulfonylmethyl) ether solution into the N6-acetyl-L-lysine methyl ester solution at 25 ℃ under the nitrogen atmosphere and under the stirring condition, heating to 65 ℃ after dropwise adding is finished, carrying out reflux reaction for 8 hours, and carrying out reduced pressure distillation to obtain hyperbranched polylysine; dissolving 0.2mol of hyperbranched polylysine in 100ml of organic solvent, dissolving 0.2mol of 1-methyl-2-propylene-1-amino methanol in 50ml of organic solvent, dropwise adding the mixture into the hyperbranched polylysine under the conditions of nitrogen atmosphere and stirring, heating to 65 ℃ after the titration is finished, carrying out closed reaction for 3 hours, and carrying out reduced pressure distillation after the reaction is finished to obtain a viscous product, namely the hyperbranched polylysine tertiary amine.
Example 2:
preparing hyperbranched polylysine tertiary amine, namely dissolving 0.5mol of N6-acetyl-L-lysine in 100ml of methanol solution at normal temperature, then placing the N6-acetyl-L-lysine solution in a closed container, performing reflux reaction for 15h under the condition of surrounding and stirring nitrogen atmosphere, and then performing reduced pressure distillation on a reaction product to obtain N6-acetyl-L-lysine methyl ester; respectively dissolving 0.3mol of N6-acetyl-L-lysine methyl ester and 0.3mol of 2-methylene-1, 4-divinyl succinate in 100ml of organic solvent, dropwise adding the 2-methylene-1, 4-divinyl succinate solution into the N6-acetyl-L-lysine methyl ester solution at 45 ℃ under the nitrogen atmosphere and under the stirring condition, heating to 70 ℃ after dropwise adding, carrying out reflux reaction for 10 hours, and carrying out reduced pressure distillation to obtain hyperbranched polylysine; dissolving 0.2mol of hyperbranched polylysine in 100ml of organic solvent, dissolving 0.2mol of 1-methyl-2-propylene-1-amino methanol in 50ml of organic solvent, dropwise adding the mixture into the hyperbranched polylysine under the conditions of nitrogen atmosphere at a certain temperature and stirring, heating to 70 ℃ after the titration is finished, carrying out closed reaction for 3 hours, and carrying out reduced pressure distillation after the reaction is finished to obtain a viscous product, namely the hyperbranched polylysine tertiary amine.
In order to further illustrate the effects of the hyperbranched polylysine tertiary amine intercalation inhibitor and the water-based drilling fluid, the hyperbranched polylysine tertiary amine intercalation inhibitor and the water-based drilling fluid prepared in the embodiments 1 and 2 are subjected to performance tests.
Second, performance test
1. Hyperbranched polylysine Tertiary amine molecular weight test
The hyperbranched polylysine tertiary amines contained in the examples were subjected to molecular weight testing using TOF-LC/MS, the results of which are shown in FIGS. 1 and 2. According to the figure 1 (taking example 1 as an example), the mass-to-charge ratio of the synthesized substances is respectively 1059.426, 1587.639, 2116.852, 2646.065, 3175.278, 3704.491, 4233.704 and the like, one proton is obtained due to positive ion scanning, the test result is consistent with the theoretically accurate molecular weight, the difference between adjacent ion peaks is 529, namely, one repeating unit is different between each ion peak, and the difference is consistent with the theoretically calculated value, so that the synthesis success of the hyperbranched polylysine tertiary amine is proved. As can be seen from FIG. 1 and FIG. 2, the intensities of the peaks are different because the reaction conditions are different and the proportion of the hyperbranched polylysine tertiary amine with different degrees of branching is also different.
2. Evaluation of environmental protection
The hyperbranched polylysine tertiary amine intercalation inhibitor as a shale intercalation inhibitor has the advantages of excellent inhibition performance, simple production process and easy biodegradation. Biodegradation of polymers refers to the phenomenon of converting them into simple inorganic substances under the action of microorganisms (fungi, molds, etc.). Biodegradability can be expressed by biochemical property (BOD5/CODcr), BOD5 is measured by an inoculation and dilution method (reference standard HJ/T505-2009 measuring dilution and inoculation method for five-day biochemical oxygen demand (BOD5) of water quality), and CODcr is measured by a potassium dichromate method (reference standard HJ/T377-2007 online automatic monitoring instrument for chemical oxygen demand (CODcr) of water quality), and the ratio is 57.1%, so that the shale inhibitor is easy to degrade, and the shale inhibitor is an environment-friendly shale inhibitor.
3. Rolling recovery test
The invention is mainly illustrated by the following specific formula of the application mode of the hyperbranched polylysine tertiary amine intercalation inhibitor. The specific formula is as follows: water, bentonite and anhydrous Na2CO3+ coating agent (KPAM) + filtrate reducer (SMP-1) + anti-collapse agent (FRH) + alkalinity regulator (CaO) + shear strength improving agent (NH-1) + weighting agent (nano barite).
One part of drilling fluid base slurry is taken as a reference group and named as base slurry, 1 percent, 2 percent and 3 percent of the hyperbranched polylysine tertiary amine intercalation inhibitor prepared by the method is added into the other 3 parts of prepared base slurry, and 3 percent of hexamethylene diamine is added into the 1 part of prepared base slurry. The base slurry is used as a blank experimental group, and the base slurry and the hexamethylene diamine are used as a control group. The inhibition performance prepared in the above examples is evaluated by rolling recovery rate, and the specific operation steps refer to oil and gas industry standard SY/T6335-1997 shale inhibitor evaluation method for drilling fluid. The higher the rolling recovery, the better the inhibition performance of the inhibitor. The results of the experiment are shown in table 1.
TABLE 1 influence of hyperbranched polylysine tertiary amine intercalation inhibitors on Rolling recovery
| Components | Recovery (%) |
| Base pulp | 24.18 |
| Base stock + 3% hexamethylenediamine | 76.47 |
| Base stock + 1% example 1 | 83.21 |
| Base stock + 2% example 1 | 86.47 |
| Base stock + 3% example 1 | 91.34 |
| Base stock + 1% example 2 | 84.76 |
| Base stock + 2% example 2 | 88.14 |
| Base stock + 3% example 2 | 92.48 |
As can be seen from Table 1, when ethylenediamine and the hyperbranched polylysine tertiary amine intercalation inhibitors obtained in different examples are used in the same proportion, the inhibition performance of the hyperbranched polylysine tertiary amine intercalation inhibitor is obviously higher than that of the conventional shale inhibitors such as hexamethylenediamine. The effect of example 2 is slightly better as seen by comparing the effects of example 1 and example 2. The influence of the inhibitor content on the rolling recovery rate indicates that the rolling recovery rate increases and the inhibition performance is better as the addition amount of the inhibitor increases.
In conclusion, the preparation method of the hyperbranched polylysine tertiary amine intercalation inhibitor provided by the invention has the advantages of stable and reliable technology and high yield, and is suitable for industrial production; the synthesized hyperbranched polylysine tertiary amine intercalation inhibitor product is non-toxic and harmless, has good water solubility, and the inhibition performance of the prepared shale hydration inhibitor is obviously improved compared with similar products, so that the shale hydration inhibitor can meet the drilling requirements of various complex well conditions, and the occurrence probability of unstable well wall caused by shale hydration dispersion is effectively reduced.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.
Claims (8)
1. The synthesis of the hyperbranched polylysine tertiary amine intercalation inhibitor is characterized in that the environment-friendly hyperbranched polylysine tertiary amine intercalation inhibitor is prepared by mixing environment-friendly hyperbranched polylysine tertiary amine and water, wherein the mass ratio of the environment-friendly hyperbranched polylysine tertiary amine in drilling fluid is 0.5-5%, the raw materials of the hyperbranched intercalation inhibitor are lysine substances containing secondary amine and sulfone substances containing olefinic bond, and the end-capping reagent is B-dimethylaminoethyl vinyl ether or 3- (ethyleneoxy) -N, N-dimethyl-1-propylamine, and the hyperbranched polylysine tertiary amine intercalation inhibitor is prepared by adopting the following steps:
s1, dissolving 0.5mol of lysine substance containing secondary amine in 100ml of methanol solution at normal temperature, then placing the lysine substance solution containing secondary amine in a closed container, refluxing and reacting for 12-14h under the condition of surrounding nitrogen atmosphere and stirring, and then distilling the reaction product under reduced pressure to obtain lysine ester;
s2, respectively dissolving 0.3mol of lysine ester and 0.3mol of ester substance containing polyene bond in 100ml of organic solvent, dropwise adding the ester substance solution containing polyene bond into the lysine ester solution at 15-30 ℃ under the nitrogen atmosphere and stirring conditions, heating to 65-75 ℃ after dropwise adding, carrying out reflux reaction for 8-10h, and carrying out reduced pressure distillation to obtain hyperbranched polylysine;
s3, dissolving 0.2mol of hyperbranched polylysine in 100ml of organic solvent, dissolving 0.2mol of end-capping reagent in 50ml of organic solvent, dropwise adding the solution into the hyperbranched polylysine solution under the conditions of nitrogen atmosphere and stirring, heating to 65-70 ℃ after the titration is finished, sealing and reacting for 3 hours, and after the reaction is finished, carrying out reduced pressure distillation to obtain a viscous product, namely the hyperbranched polylysine tertiary amine.
2. The hyperbranched polylysine tertiary amine intercalation inhibitor of claim 1, wherein the lysine species containing secondary amines of step S1 is one of N6-acetyl-L-lysine and N epsilon-formyl-L-lysine.
3. The hyperbranched polylysine tertiary amine intercalation inhibitor of claim 1, wherein the ester species containing a polyethylenic bond is one of bis (vinylsulfonylmethyl) ether and bis (vinylsulfonyl) propanol.
4. The hyperbranched polylysine tertiary amine intercalation inhibitor according to claim 1, wherein the organic solvent in steps S2, S3, and S4 is one of absolute methanol and absolute ethanol.
5. The hyperbranched polylysine tertiary amine intercalation inhibitor of claim 1, wherein the capping reagent is one of 1-methyl-2-propene-1-aminomethanol, 1-ethyl-2-propene-1-aminomethanol.
6. The hyperbranched polylysine tertiary amine intercalation inhibitor according to claim 1, wherein the step S2 dropping time is controlled to be 35-45min, the step S3 dropping time is controlled to be 40-50min, and the step S4 dropping time is controlled to be 40-50 min.
7. The hyperbranched polylysine tertiary amine intercalation inhibitor according to claim 1, wherein the reduced pressure distillation temperature of steps S1, S2, S3, S4 is 80-100 ℃ and the absolute vacuum is less than 3000 Pa.
8. The water-based drilling fluid of claim 1, wherein the bentonite is added in an amount of 2-4 parts by weight based on 100 parts by weight of water, and the anhydrous Na is2CO3The addition amount of the NaOH is 0.3 to 0.4 weight part, the addition amount of the NaOH is 0.1 to 0.3 weight part, the coating agent (KPAM) is added in an amount of 0.01-0.03 parts by weight, the salt-resistant agent (PAC-LV) is added in an amount of 0.3-0.8 parts by weight, the addition amount of the filtrate reducer (SMP-1) is 5 to 6 parts by weight, the addition amount of the anti-collapse agent (FRH) is 3 to 5 parts by weight, the addition amount of the anti-seize lubricant (FK-10) is 4 to 5 parts by weight, the addition amount of the alkalinity regulator (CaO) is 0.3 to 0.5 part by weight, the addition amount of the stripping and cutting agent (NH-1) is 1 to 2 weight parts, the addition amount of the inhibitor (hyperbranched polylysine tertiary amine) is 0.5 to 5 weight parts, the weight additive (nano barite) is added in an amount of 0-200 parts by weight (density is adjustable).
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