CN113416525A - Environment-friendly polyether tertiary amine as shale surface hydration inhibitor - Google Patents
Environment-friendly polyether tertiary amine as shale surface hydration inhibitor Download PDFInfo
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Abstract
The invention discloses an environment-friendly polyether tertiary amine as a shale surface hydration inhibitor, belonging to the technical field of oil and gas field drilling. The shale surface hydration inhibitor prepared from the environment-friendly polyether tertiary amine is prepared by mixing the environment-friendly polyether tertiary amine and water, wherein the mass ratio of the environment-friendly polyether tertiary amine in the shale surface hydration inhibitor is 0.5-5%. Compared with the similar surface hydration inhibitor, the shale surface hydration inhibitor prepared from the environment-friendly polyether tertiary amine provided by the invention has the advantages of obviously improved inhibition performance, excellent biodegradability, simple synthesis method and easy industrial popularization and application.
Description
Technical Field
The invention relates to the technical field of oil and gas field drilling, in particular to an environment-friendly polyether tertiary amine serving as a shale surface hydration inhibitor.
Background
The development of shale gas becomes an important measure for guaranteeing the energy safety of China, the burial depth of shale in China is about 65% to be more than 3500m, and the proportion of deep shale gas resource amount of over 3500m in the south of Sichuan basin (called Chuannan area for short) to the total resource amount of the whole Chuannan area is up to 86.5%. Therefore, deep shale gas has become a main field of future shale gas yield increase. In the south China, shale gas dominant reservoir takes hard and brittle shale illite as a main material, however, the borehole wall collapse of hard and brittle shale is an important technical bottleneck for restricting the successful transfer of oil and gas resource strategies to deep strata in China, and more than 70% of borehole problems in shale gas drilling are caused by shale instability. Most shale gas horizontal wells finished at home and abroad are drilled by adopting an oil-based drilling fluid system, the oil-based drilling fluid has the advantages of good stability of well walls and strong inhibition capability, and the oil-based drilling fluid accounts for about 90 percent. However, the oil-based drilling fluid has the problems of environmental pollution, high cost, high circulation loss tendency and the like, and the oil-based drilling fluid becomes a great obstacle to the industrial development of deep shale gas in China. In order to comply with the development process of large-scale deep shale gas and solve the problems, the drilling of deep shale gas wells by using water-based drilling fluid which is environment-friendly, low in cost and equivalent to oil base in performance is a necessary development trend.
The inhibition of the shale inhibitor determines the inhibition of the water-based drilling fluid, and the inhibitor at the present stage achieves the effect of inhibiting the hydration of clay minerals mainly by inhibiting the hydration of interlayer cations of the clay minerals. However, for shale containing illite as a main component, the hydration is surface hydration, so that the development of an inhibitor capable of inhibiting the surface hydration of the shale is an urgent problem to be solved.
Disclosure of Invention
In view of the defects of the existing surface hydration inhibitor, the invention provides an environment-friendly polyether tertiary amine as a shale surface hydration inhibitor, and the inhibitor contains tertiary amine groups and ether bonds in molecules, has better environment-friendly performance, and can enable clay minerals to achieve the effects of interface modification and wetting reversion so as to inhibit the shale surface hydration. Compared with similar products, the surface hydration inhibition performance provided by the invention is obviously improved, the drilling requirements of various complex well conditions can be completely met, and the synthetic process is simple, environment-friendly, high in yield, low in production cost and suitable for industrial production.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the shale surface hydration inhibitor is prepared by mixing environment-friendly polyether tertiary amine and water, wherein the mass ratio of the environment-friendly polyether tertiary amine is 0.5-3%, and the environment-friendly polyether tertiary amine is synthesized by taking an ether amine compound, a diene compound and an ether compound containing a monoethene bond as raw materials.
The structural general formula of the ether amine compound is as follows: h2N-(CH2)n-O-(CH2) n-NH-R or H2N-(CH2)n-NH-(CH2) n-O-R, n ═ 0,1,2,3,4,5, R is methyl, ethyl, propyl, isopropyl, butyl, isobutyl, sec-butyl, tert-butyl, or the like. The following substances are mainly included but not limited to all substances according to the structural general formula: n '- (2-methoxyethyl) propane-1, 3-diamine, N' - (3-methoxypropyl) ethane-1, 2-diamine, N1- (3-methoxypropyl) -1, 3-propanediamine, 2- [2- (2-aminoethoxy) ethylamino]Ethanol, 2- [2- (2-aminoethylamino) ethoxy]Ethanol, N- [3- [ (2-ethylhexyl) oxy group]Propyl radical]Propane-1, 3-diamine, N- [3- (isooctyloxy) propyl]Propane-1, 3-diamine, N- [3- [ (2-ethylhexyl) oxy group]Propyl radical]Propane-1, 3-diamine, N- [3- (isooctyloxy) propyl]Propane-1, 3-diamine, N- [3- (isononyloxy) propyl]Propane-1, 3-diamine.
The diene compound is one of diallyl methylamine and N, N-diallyl hydroxylamine.
The structural general formula of the ether compound containing the monoethylene bond is as follows: CH (CH)2CH-(CH2)n-O-(CH2) n-R, wherein n is 0,1,2,3,4,5, R is selected from methyl, ethylAnd the like, propyl, isopropyl, butyl, isobutyl, sec-butyl, tert-butyl and the like.
The synthesis steps of the environment-friendly polyether tertiary amine shale surface hydration inhibitor are as follows:
s1, mixing the components in a molar ratio of 1: (1-1.2) Etheramine Compound and diene bond Compound were dissolved in an organic solvent, respectively, to obtain solution A and solution B.
S2, dropwise adding the solution B into the solution A at the first temperature, raising the temperature to the second temperature after dropwise adding, and carrying out reflux reaction for 6-12 h. After the reaction is complete, the product is rotary evaporated to a branched polyetheramine.
S2, mixing the components in a molar ratio of 1: the branched polyetheramine obtained in S1 of (1-1.2) and the ether-based compound having a monoethylene bond were sufficiently dissolved in an organic solvent to obtain a solution C and a solution D.
S4, dropwise adding the solution D into the solution C under the first temperature condition, and after dropwise adding is finished, raising the temperature to a second temperature for reflux reaction for 6-12 h. After the reaction is finished, the product is subjected to reduced pressure distillation, washing, drying and repeating the operation for 3 times to obtain the branched polyether tertiary amine.
The dripping time is controlled within 35-50 min.
The first temperature is 25-40 ℃, and the second temperature is 80-100 ℃.
The organic solvent is absolute ethyl alcohol or absolute methyl alcohol, wherein the mass percentage concentration of ether amine compounds and silane compounds containing olefinic bonds in the organic solvent is 0.5-5%.
The detergent is acetone, and the rotary evaporation temperature is 55-80 ℃.
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 environment-friendly polyether tertiary amine, has stable performance and strong adaptability, has obviously improved inhibition performance compared with similar products, and can meet the drilling requirements of various complex well conditions.
Drawings
FIG. 1 is a chemical structural diagram of environmentally friendly polyether tertiary amine S1 obtained in example 1;
FIG. 2 is the chemical structural diagram of the environmentally friendly polyether tertiary amine S2 obtained in example 2;
FIG. 3 is a diagram showing a distribution of molecular weight of environmentally friendly polyether tertiary amine S1 obtained in example 1;
FIG. 4 is a molecular weight distribution diagram of environmentally friendly polyether tertiary amine S2 obtained in example 2.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
Example 1:
the method takes N' - (2-methoxyethyl) propane-1, 3-diamine, diallyl methylamine and vinyl methyl ether as raw materials, and comprises the following specific operation steps:
0.1mol of N' - (2-methoxyethyl) propane-1, 3-diamine and 0.12mol of diallylmethylamine were weighed out and dissolved in 100ml of absolute ethanol, respectively. Setting the temperature to be 30 ℃, dropwise adding the diallylmethylamine solution into the diethylenetriamine solution, raising the temperature to 95 ℃ after the dropwise adding is finished, and carrying out condensation reflux reaction for 10 hours. And after the reaction is finished, the product is subjected to rotary evaporation at the temperature of 70 ℃ to obtain the branched polyether amine.
0.1mol of the branched polyetheramine obtained in the preceding step and 0.12mol of vinyl methyl ether were weighed out and dissolved in 100ml of absolute ethanol. Setting the temperature to be 30 ℃, dropwise adding the vinyl methyl ether solution into the branched polyether amine solution, raising the temperature to 95 ℃ after dropwise adding, and carrying out condensation reflux reaction for 10 hours. And after the reaction is finished, performing rotary evaporation on the product at 70 ℃, washing with acetone, and performing rotary evaporation to obtain the branched polyether tertiary amine S1, wherein the chemical structural formula of the branched polyether tertiary amine S1 is shown in figure 1.
Wherein, R1 ═ - (CH2)3-，R2＝-(CH2)2OCH3，R＝-(CH2)2O(CH2)2CH3
Example 2:
the method takes N1- (3-methoxy propyl) -1, 3-propane diamine, N, N-diallyl hydroxylamine and N-propyl vinyl ether as raw materials, and comprises the following specific operation steps:
0.1mol of N1- (3-methoxypropyl) -1, 3-propanediamine and 0.12mol of N, N-diallylhydroxylamine were weighed out and dissolved in 100ml of absolute ethanol. Setting the temperature to be 30 ℃, dropwise adding the N, N-diallyl hydroxylamine solution into the N1- (3-methoxypropyl) -1, 3-propane diamine solution, raising the temperature to 95 ℃ after dropwise adding, and carrying out condensation reflux reaction for 10 hours. And after the reaction is finished, carrying out rotary evaporation on the product at the temperature of 70 ℃ to obtain the branched polyether amine.
0.1mol of the branched polyetheramine obtained in the preceding step and 0.12mol of n-propyl vinyl ether were weighed out and dissolved in 100ml of absolute ethanol. Setting the temperature to be 30 ℃, dropwise adding the n-propyl vinyl ether solution into the branched polyetheramine solution, raising the temperature to 95 ℃ after dropwise adding, and carrying out condensation reflux reaction for 10 hours. And after the reaction is finished, performing rotary evaporation on the product at 70 ℃, washing with acetone, and performing rotary evaporation to obtain the branched polyether tertiary amine S1, wherein the chemical structural formula of the branched polyether tertiary amine S1 is shown in figure 2.
Wherein R is1＝-(CH2)3-，R2＝-(CH2)3OCH3，R＝R2＝-(CH2)2OCH3
1. Molecular weight measurement
The environmental-friendly branched polyether tertiary amine included in the examples was subjected to a molecular weight test using TOF-LC/MS, and the test results are shown in FIGS. 3 and 4. According to the results of polymer mass spectrometry (taking example 1 as an example), the molecular weights of the three peaks are respectively 375.592, 618.955, 862.314, 1105.674, 1349.051, 1598.392, 1841.754 and the like, the peaks are ionic peaks of the environment-friendly branched polyether tertiary amine with different branching degrees, the difference between adjacent ionic peaks is 243, namely, each ionic peak is different by one repeating unit and is matched with the theoretical calculation value. Therefore, the environment-friendly branched polyether tertiary amine is proved to be successfully synthesized.
2. Biochemical performance testing
Biochemical properties (BOD5/CODcr) are used herein to denote the biodegradation rate, and BOD is determined by the inoculation and dilution method5(reference standard HJ/T505-2009), and CODcr was determined by the potassium dichromate method (reference standard YJ/T377-2007). According to a series of standards of international organization for economic collaboration and development (OCED) on the biodegradability of chemicals, the closed bottle method (301D) indicates that the chemicals are considered to be easily biodegradable substances when the biodegradation rate of the chemicals is not less than 60%. The biodegradability of the environment-friendly polyether tertiary amines S1 and S2 obtained in examples 1 and 2 is tested, and the test results are shown in Table 1:
TABLE 1 BOD5Results of the CODcr test
| Shale surface hydration inhibitor | BOD5(mg·L-1) | CODcr(mg·L-1) | BOD5/CODcr(％) |
| Environment-friendly polyether tertiary amine S1 | 113 | 167 | 67.66 |
| Environment-friendly polyether tertiary amine S2 | 115 | 166 | 69.28 |
As can be seen from Table 1, BOD of the surface hydration inhibitors obtained in examples 1 and 25The values of/CODcr are all larger than 60 percent, which shows that the shale surface hydration inhibitor has good biodegradability and can be decomposed through biodegradation, belongs to an environment-friendly shale surface hydration inhibitor and responds to the national requirement on environmental protection.
3. Rolling recovery test
The environmentally-friendly polyether tertiary amine obtained in examples 1 and 2 and clean water are prepared into shale inhibitors and conventional shale inhibitors (conventional polyamine inhibitors and hexamethylenediamine inhibitors are selected) according to a proportion (the mass ratio of the environmentally-friendly polyether tertiary amine is 1%, 2%, 3%, 4% and 5%) for comparison experiments, and the clean water is used as a reference. 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 2.
TABLE 2 Effect of surface hydration inhibitors on Rolling recovery
| Components | Recovery (%) |
| Clean water | 19.54 |
| 1% hexamethylene diamine | 28.32 |
| 1% of polyamine | 44.60 |
| 1% of the ring S1 obtained in example 1Shape-maintaining polyether tertiary amine | 73.26 |
| 2% Environment-friendly polyether Tertiary amine S1 obtained in example 1 | 75.04 |
| 3% Environment-friendly polyether Tertiary amine S1 obtained in example 1 | 77.92 |
| 4% Environment-friendly polyether Tertiary amine S1 from example 1 | 80.28 |
| 5% of the environmentally friendly polyether tertiary amine S1 obtained in example 1 | 82.44 |
| 1% of the environmentally friendly polyether tertiary amine S2 obtained in example 2 | 73.99 |
| 2% Environment-friendly polyether Tertiary amine S2 obtained in example 2 | 74.83 |
| 3% of the environmentally friendly polyether tertiary amine S2 obtained in example 2 | 77.56 |
| 4% Environment-friendly polyether Tertiary amine S2 from example 2 | 80.21 |
| 5% of the environmentally friendly polyether tertiary amine S2 obtained in example 2 | 83.07 |
The results of the influence of different surface hydration inhibitors on the rolling recovery rate in table 2 show that the inhibition performance of the environment-friendly polyether tertiary amine is obviously higher than that of the conventional shale inhibitors such as hexamethylene diamine, polyamine and the like when the ethylene diamine, the polyamine and the environment-friendly polyether tertiary amine obtained in different embodiments are in the same proportion. The inhibition effect of the environment-friendly polyether tertiary amine surface hydration inhibitor is obviously higher than that of the conventional shale inhibitor. 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 environment-friendly polyether tertiary amine provided by the invention has the advantages of stable and reliable technology, high yield and suitability for industrial production; the synthesized environment-friendly polyether tertiary amine product is non-toxic and harmless, has good water solubility, and the inhibition performance of the prepared shale surface hydration inhibitor is obviously improved compared with similar products, so that the shale surface hydration inhibitor can meet the drilling requirements of various complex well conditions, and the occurrence probability of unstable well walls 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 (9)
1. The shale surface hydration inhibitor is characterized by being prepared by mixing environment-friendly polyether tertiary amine and water, wherein the mass ratio of the environment-friendly polyether tertiary amine is 0.5-5%, and the environment-friendly polyether tertiary amine is synthesized by taking an ether amine compound, a diene compound and an ether compound containing a monoethene bond as raw materials.
2. The inhibitor of claim 1, wherein the ether amine compound has the general structural formula: h2N-(CH2)n-O-(CH2) n-NH-R or H2N-(CH2)n-NH-(CH2) n-O-R, n ═ 0,1,2,3,4,5, R is methyl, ethyl, propyl, isopropyl, butyl, isobutyl, sec-butyl, tert-butyl, and the like, and includes, but is not limited to, all of the following materials conforming to the general structural formula: n '- (2-methoxyethyl) propane-1, 3-diamine, N' - (3-methoxypropyl) ethane-1, 2-diamine, N1- (3-methoxypropyl) -1, 3-propanediamine, 2- [2- (2-aminoethoxy) ethylamino]Ethanol, 2- [2- (2-aminoethylamino) ethoxy]Ethanol, N- [3- [ (2-ethylhexyl) oxy group]Propyl radical]Propane-1, 3-diamine, N- [3- (isooctyloxy) propyl]Propane-1, 3-diamine, N- [3- [ (2-ethylhexyl) oxy group]Propyl radical]Propane-1, 3-diamine, N- [3- (isooctyloxy) propyl]Propane-1, 3-diamine, N- [3- (isononyloxy) propyl]Propane-1, 3-diamine.
3. The inhibitor according to claim 1, wherein the diene compound is: one of diallylmethylamine and N, N-diallylhydroxylamine.
4. The inhibitor according to claim 1, wherein the ether compound containing a monoethylene bond has a general structural formula: CH (CH)2CH-(CH2)n-O-(CH2) n-R, wherein n is 0,1,2,3,4,5, R is selected from methyl, ethyl, propyl, isopropyl, butyl, isobutyl, sec-butyl, tert-butyl and the like.
5. The preparation method of claim 1, wherein the environmentally friendly polyether tertiary amine shale surface hydration inhibitor is synthesized by the following steps:
s1, mixing the components in a molar ratio of 1: respectively dissolving the ether amine compound and the diene bond compound of (1-1.2) in an organic solvent to obtain a solution A and a solution B;
s2, dropwise adding the solution B into the solution A at the first temperature, raising the temperature to the second temperature after dropwise adding is finished, carrying out reflux reaction for 6-12h, and carrying out rotary evaporation on the product to obtain branched polyetheramine after the reaction is finished;
s2, mixing the components in a molar ratio of 1: (1-1.2) the branched polyetheramine obtained in S1 and the ether-based compound having a monoethylene bond are sufficiently dissolved in an organic solvent to obtain a solution C and a solution D;
s4, dropwise adding the solution D into the solution C under the first temperature condition, raising the temperature to a second temperature after dropwise adding is finished, carrying out reflux reaction for 6-12h, and after the reaction is finished, carrying out reduced pressure distillation on the product, washing, drying and repeating the operation for 3 times to obtain the branched polyether tertiary amine.
6. The synthesis method of claim 5, wherein the dropping time is controlled to be 35-50 min.
7. The method of synthesis of claim 5, wherein the first temperature is 25-40 ℃ and the second temperature is 80-100 ℃.
8. The synthesis method according to claim 5, wherein the organic solvent is absolute ethyl alcohol or absolute methyl alcohol, and the mass percentage of the raw material in the organic solvent is 1.0-5.0%.
9. The synthesis method according to claim 5, wherein the detergent is acetone and the rotary evaporation temperature is 55-80 ℃.
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