CN111323412A - On-site monitoring method for content of amino polyether in drilling fluid filtrate - Google Patents
On-site monitoring method for content of amino polyether in drilling fluid filtrate Download PDFInfo
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Abstract
The invention provides a field monitoring method for the content of amino polyether in drilling fluid filtrate, which adopts a conventional titration analysis method, does not need special instruments and equipment, is simple, convenient and quick, and is suitable for field monitoring of drilling wells. The method solves the problem that the content of the amino polyether is difficult to directly measure due to complex components and multiple interference factors of the drilling fluid filtrate, fills the gap of monitoring the content of the amino polyether in the drilling fluid filtrate, and has important significance for guiding field construction.
Description
Technical Field
The invention belongs to the technical field of chemical analysis of drilling fluid, and particularly relates to a field monitoring method for the content of amino polyether in drilling fluid filtrate.
Background
The amino polyether is also called as polyether amine, and is a polymer with a polyether structure as a main chain and amino as a terminal active functional group. In recent years, the amino polyether is increasingly applied to drilling fluid, can be independently used as a drilling fluid inhibitor or an anti-collapse agent, and can also form an amino polyether drilling fluid system for use.
During drilling, the drilling fluid is in a dynamic state, and the content of the treating agent is also a cyclic process of consumption-supplement-consumption-supplement. After the amino polyether is added into the drilling fluid, free amino polyether in a liquid phase, namely the amino polyether in the filtrate, can play a role in stabilizing the well wall, so that the important role can be fully played only by monitoring the content of the filtrate in real time and replenishing the amino polyether in due time. However, since there is no method to monitor the content, the field constructors mostly rely on personal feelings to supplement the content in the maintenance process, if the content is less than the content, the inhibition effect cannot be fully exerted, so that the well wall is unstable, and if the content is more than the content, the blind use is caused, so that the cost is increased. It is therefore desirable to provide a method for on-site monitoring of the amine-based polyether content of drilling fluid filtrate.
The patent application No. 201410299336.2 discloses a method for determining the adsorption performance of organic drilling fluid treating agent, which can obtain the amount of organic drilling fluid treating agent by directly determining the content of carbon and/or nitrogen elements. However, the method is only suitable for the situation that the drilling fluid only contains one organic treating agent, and the drilling fluid used in a drilling site cannot contain only one organic treating agent of the amino polyether, so that the method is not suitable.
The patent application No. 200910273114.2 discloses a method for rapidly and accurately determining the content of fatty amine in a powdery anti-caking agent, which adopts a potentiometric titration method to titrate the content of fatty amine by perchloric acid-glacial acetic acid standard solution, but the potentiometric titration method is used in a potentiometric titrator, a drilling site is not equipped generally, and the components of drilling fluid filtrate are complex and interfere with the sensitivity of an electrode.
Patent application No. 201710482119.0 discloses a qualitative determination method for determining whether a nitro compound fertilizer oil body anticaking agent ingredient is correct, which uses bromocresol green as an indicator, hydrochloric acid-isopropanol as a titration solution to titrate the amine value of the nitro compound fertilizer oil body anticaking agent, and utilizes the principle that hydrochloric acid titrates alkaline amine, but the components of the filtrate of the drilling fluid are complex, and the filtrate of the drilling fluid often contains various amine-containing treating agents except amine polyether, and also contains free alkali such as NaOH, and the components of the treating agents are in a constantly changing state, so that the content of the amine polyether in the filtrate can not be directly titrated.
The content determination of the amine-based polyether in the drilling fluid filtrate has the following difficulties: on one hand, as the well drilling construction site is mostly in the fields, grasslands, deserts and other places far away from the smoke of people, and the field is provided with limited instruments and equipment, the analysis methods such as chromatographic analysis, spectrophotometer method and the like which need special instruments are not suitable for measuring the free content of the amino polyether in the well drilling site, so that the simple and easy analysis method is preferably adopted. On the other hand, since the drilling fluid system is a complex system composed of a plurality of raw materials and treating agents, the components of the drilling fluid system can be as many as ten kinds, and the components are constantly changing, and the following raw materials are commonly used: bentonite, barite, and the like; commonly used inorganic treating agents are: sodium hydroxide, sodium carbonate, calcium carbonate, sodium chloride, ammonium chloride, potassium sulfate, and the like; commonly used organic treating agents are: sodium carboxymethyl cellulose with different molecular weights, polyanionic cellulose, polyacrylamide potassium salt, polymer fluid loss additive, hydrolyzed polyacrylonitrile ammonium salt, macromolecular polyacrylamide, xanthan gum, carboxymethyl starch, amino polyether, polymeric alcohol, lignite, resin and the like, wherein the influence of inorganic bases such as sodium hydroxide and the like and various organic treating agents containing amino groups is measured; meanwhile, the filtrate also contains color due to colored treating agents such as lignite, resin and the like, and the endpoint judgment is influenced during titration. The greatest difficulty in determining the content of amine-based polyethers in drilling fluid filtrates is therefore the elimination of interference from other components.
Therefore, the invention discloses a method for rapidly monitoring the content of the amine polyether in the filtrate of the drilling fluid, which can eliminate the interference of other chemical components and is convenient for a drilling site.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a method for monitoring the content of aminopolyether in a drilling fluid filtrate on site, wherein the content of aminopolyether in the drilling fluid filtrate can be determined by a titration method, and interference of other chemical components can be eliminated, so that the method is convenient and rapid.
The invention provides a field monitoring method for the content of amino polyether in drilling fluid filtrate, which comprises the following steps:
A) drawing a standard curve:
taking a plurality of parts of blank drilling fluid filtrate, and adding amino polyether with different mass to obtain amino polyether standard solutions with different concentrations, wherein the blank drilling fluid filtrate is drilling fluid filtrate without amino polyether;
respectively mixing and stirring the amino polyether standard solutions with different concentrations and an alcohol solvent, standing and filtering to obtain filtrate;
taking the filtrate, adding a phenolphthalein indicator, titrating the filtrate to be colorless by using a hydrochloric acid-alcohol solvent solution, then adding a bromophenol blue indicator, titrating the filtrate by using a hydrochloric acid-alcohol solvent solution until the filtrate turns yellow from blue, recording the volume of the hydrochloric acid-alcohol solvent solution consumed in the process from blue to yellow, calculating the amount of substances consuming hydrochloric acid according to the concentration of the hydrochloric acid-alcohol solvent solution, and drawing a linear relation standard curve of the concentration of the amino polyether and the amount of the substances consuming hydrochloric acid;
B) and (3) determining the content of the amino polyether in the filtrate of the drilling fluid to be detected:
mixing and stirring the filtrate of the drilling fluid to be detected and an alcohol solvent, standing and filtering to obtain filtrate;
and taking the filtrate, adding a phenolphthalein indicator, titrating with a hydrochloric acid-alcohol solvent solution until the filtrate is colorless, adding a bromophenol blue indicator, titrating with a hydrochloric acid-alcohol solvent solution until the filtrate turns yellow from blue, recording the volume of the hydrochloric acid-alcohol solvent solution consumed in the process from blue to yellow, calculating the amount of hydrochloric acid consumed by the filtrate according to the concentration of the hydrochloric acid-alcohol solvent solution, and calculating the content of the amino polyether in the filtrate of the drilling fluid according to the linear relation standard curve obtained in the step A).
Preferably, the drilling fluid is a water-based drilling fluid comprising: polymer drilling fluid, polysulfonate drilling fluid, saturated brine drilling fluid, potassium chloride drilling fluid, polymer potassium chloride drilling fluid and amino polyether drilling fluid.
Preferably, the concentration of the amine-based polyether standard solution with different concentrations is 0g/L, 10g/L, 20g/L and 30 g/L.
Preferably, the mass concentration of the phenolphthalein indicator is 1%, and the mass concentration of the bromophenol blue indicator is 2%.
Preferably, the alcohol solvent in step a) and the alcohol solvent in step B) are the same alcohol solvent, and the alcohol solvent is selected from ethanol, isopropanol or propanol.
Preferably, in the step A), the volume ratio of the alcohol solvent to the amine-based polyether standard solution is more than 7: 3;
in the step B), the volume ratio of the alcohol solvent to the filtrate of the drilling fluid to be detected is more than 7: 3;
the volume ratio of the alcohol solvent to the amino polyether standard solution is the same as the volume ratio of the alcohol solvent to the drilling fluid filtrate to be measured.
Preferably, in the step A), the concentration of the hydrochloric acid-alcohol solvent solution used in the process of titration to colorless is 0.08-0.14 mol/L; the concentration of a hydrochloric acid-alcohol solvent solution used in the process of titrating until the blue color turns yellow is 0.08-0.14 mol/L;
in the step B), the concentration of a hydrochloric acid-alcohol solvent solution used in the process of titration to colorless is 0.08-0.14 mol/L; the concentration of the hydrochloric acid-alcohol solvent solution used in the process of titrating until the blue color turns yellow is 0.08-0.14 mol/L.
Preferably, in the step A), the standing time is 20-40 min, and the temperature is 25 +/-5 ℃;
in the step B), the standing time is 20-40 min, and the temperature is 25 +/-5 ℃.
Preferably, the amine-based polyether is a polymer with a polyether main chain and amine-based terminal active functional groups, and the number average molecular weight of the polymer is less than 1000.
Compared with the prior art, the invention provides a field monitoring method for the content of amino polyether in drilling fluid filtrate, which comprises the following steps: A) drawing a standard curve: taking a plurality of parts of blank drilling fluid filtrate, and adding amino polyether with different mass to obtain amino polyether standard solutions with different concentrations, wherein the blank drilling fluid filtrate is drilling fluid filtrate without amino polyether; respectively mixing and stirring the amino polyether standard solutions with different concentrations and an alcohol solvent, standing and filtering to obtain filtrate; taking the filtrate, adding a phenolphthalein indicator, titrating the filtrate to be colorless by using a hydrochloric acid-alcohol solvent solution, then adding a bromophenol blue indicator, titrating the filtrate by using a hydrochloric acid-alcohol solvent solution until the filtrate turns yellow from blue, recording the volume of the hydrochloric acid-alcohol solvent solution consumed in the process from blue to yellow, calculating the amount of substances consuming hydrochloric acid according to the concentration of the hydrochloric acid-alcohol solvent solution, and drawing a linear relation standard curve of the concentration of the amino polyether and the amount of the substances consuming hydrochloric acid; B) and (3) determining the content of the amino polyether in the filtrate of the drilling fluid to be detected: mixing and stirring the filtrate of the drilling fluid to be detected and an alcohol solvent, standing and filtering to obtain filtrate; and taking the filtrate, adding a phenolphthalein indicator, titrating with a hydrochloric acid-alcohol solvent solution until the filtrate is colorless, adding a bromophenol blue indicator, titrating with a hydrochloric acid-alcohol solvent solution until the filtrate turns yellow from blue, recording the volume of the hydrochloric acid-alcohol solvent solution consumed in the process from blue to yellow, calculating the amount of hydrochloric acid consumed by the filtrate according to the concentration of the hydrochloric acid-alcohol solvent solution, and calculating the content of the amino polyether in the filtrate of the drilling fluid according to the linear relation standard curve obtained in the step A). The invention adopts a conventional titration analysis method, does not need special instruments and equipment, is simple, convenient and quick, and is suitable for drilling site monitoring. The invention adopts a method of adding an alcohol solvent into the filtrate of the drilling fluid for treatment, thereby eliminating the interference of an inorganic treating agent and a macromolecular treating agent in the filtrate and simultaneously eliminating the interference of the color of the filtrate; hydroxyl and amino are respectively titrated by adopting a method of double indicator titration of a phenolphthalein indicator and a bromophenol blue indicator, so that the interference of free hydroxyl is eliminated, and the content of amino polyether in the filtrate of the drilling fluid is determined. The recovery rate of the added standard is more than 92%, and the relative standard deviation is less than 5%, which indicates that the monitoring method is feasible and has better reproducibility. The problem that the content of the amino polyether is difficult to directly measure due to the complex components of the drilling fluid filtrate and a plurality of interference factors is solved. The method fills the gap of monitoring the content of the amino polyether in the filtrate of the drilling fluid, can timely master the change condition of the effective content of the amino polyether in the drilling fluid on site, is beneficial to timely maintenance and supplement of drilling fluid engineers on site, and has important significance for guiding site construction.
Drawings
FIG. 1 is a graph of the linear relationship between the content of aminopolyether I and the consumption of hydrochloric acid;
FIG. 2 is a graph showing the linear relationship between the content of aminopolyether II and the consumption of hydrochloric acid;
FIG. 3 is a linear plot of aminopolyether III content versus hydrochloric acid consumption.
Detailed Description
The invention provides a field monitoring method for the content of amino polyether in drilling fluid filtrate, which comprises the following steps:
A) drawing a standard curve:
taking a plurality of parts of blank drilling fluid filtrate, and adding amino polyether with different mass to obtain amino polyether standard solutions with different concentrations, wherein the blank drilling fluid filtrate is drilling fluid filtrate without amino polyether;
respectively mixing and stirring the amino polyether standard solutions with different concentrations and an alcohol solvent, standing and filtering to obtain filtrate;
taking the filtrate, adding a phenolphthalein indicator, titrating the filtrate to be colorless by using a hydrochloric acid-alcohol solvent solution, then adding a bromophenol blue indicator, titrating the filtrate by using a hydrochloric acid-alcohol solvent solution until the filtrate turns yellow from blue, recording the volume of the hydrochloric acid-alcohol solvent solution consumed in the process from blue to yellow, calculating the amount of substances consuming hydrochloric acid according to the concentration of the hydrochloric acid-alcohol solvent solution, and drawing a linear relation standard curve of the concentration of the amino polyether and the amount of the substances consuming hydrochloric acid;
B) and (3) determining the content of the amino polyether in the filtrate of the drilling fluid to be detected:
mixing and stirring the filtrate of the drilling fluid to be detected and an alcohol solvent, standing and filtering to obtain filtrate;
and taking the filtrate, adding a phenolphthalein indicator, titrating with a hydrochloric acid-alcohol solvent solution until the filtrate is colorless, adding a bromophenol blue indicator, titrating with a hydrochloric acid-alcohol solvent solution until the filtrate turns yellow from blue, recording the volume of the hydrochloric acid-alcohol solvent solution consumed in the process from blue to yellow, calculating the amount of hydrochloric acid consumed by the filtrate according to the concentration of the hydrochloric acid-alcohol solvent solution, and calculating the content of the amino polyether in the filtrate of the drilling fluid according to the linear relation standard curve obtained in the step A).
In the present invention, the drilling fluid is a water-based drilling fluid comprising: polymer drilling fluid, polysulfonate drilling fluid, saturated brine drilling fluid, common brine drilling fluid, potassium chloride drilling fluid, polymer potassium chloride drilling fluid and amino polyether drilling fluid.
In some embodiments of the invention, the drilling fluid base formulation is: 4 percent of prehydrated bentonite slurry, 0.7 percent of hydrolyzed polyacrylonitrile ammonium salt, 0.3 percent of polyacrylamide, 0.3 percent of low-viscosity emulsion polymer, 0.3 percent of high-viscosity emulsion polymer, 2 percent of superfine calcium carbonate, 1 percent of oil-soluble temporary plugging agent, 0.7 percent of emulsifier, 4 percent of crude oil, 2 percent of amino polyether and the balance of water, wherein the concentrations in the formula are mass concentrations.
In other embodiments of the present invention, the drilling fluid base formulation: 4 percent of prehydrated bentonite slurry, 0.5 percent of hydrolyzed polyacrylonitrile ammonium salt, 0.3 percent of polyacrylamide, 0.5 percent of low-viscosity polyanionic cellulose, 0.3 percent of low-viscosity emulsion polymer, 2 percent of superfine calcium carbonate, 2 percent of asphalt powder, 0.2 percent of chemical cleaning agent, 0.8 percent of sodium hydroxide, 25 percent of sodium chloride, 1 percent of amino polyether and the balance of water, wherein the concentrations in the formula are mass concentrations.
In other embodiments of the present invention, the drilling fluid base formulation: 4 percent of prehydrated bentonite slurry, 0.4 percent of polymer fluid loss additive, 0.3 percent of low-sodium carboxymethyl cellulose, 2 percent of sulfonated phenolic resin, 2 percent of sulfonated lignite, 0.12 percent of NaOH, 2.5 percent of amino polyether and the balance of water, wherein the concentrations in the formula are mass concentrations.
According to the invention, the blank drilling fluid filtrate is selected as the solution for dissolving the amino polyether to draw the standard curve, the blank drilling fluid filtrate is the drilling fluid filtrate without adding the amino polyether during construction, and when the amino polyether standard solution is prepared, the blank drilling fluid filtrate is used as the solvent instead of the aqueous solution, and part of small and medium molecular weight treating agent is dissolved in the filtrate after the drilling fluid filtrate is treated by the alcohol solvent to influence the determination, so that the blank drilling fluid filtrate is used during drawing the standard curve, the system error is eliminated, and the accuracy of the result is improved.
In the invention, the amino polyether is called as polyether amine, and is a polymer with a polyether structure as a main chain and amino as a terminal active functional group. The kind of the amine-based polyether is not particularly limited in the present invention, and amine-based polyethers known to those skilled in the art to be useful as drilling fluid inhibitors or anti-sloughing agents are all possible. The amido polyether is a polymer with a polyether structure as a main chain and an amido-containing active functional group at the tail end, and the number average molecular weight is less than 1000.
In some embodiments of the present invention, the amine-based polyether has a number average molecular weight of about 230 and has the following structural formula:
in other embodiments of the present invention, the amine-based polyether is a primary amino-terminated polypropylene oxide compound containing three primary amine groups and having the following structural formula:
in other embodiments of the present invention, the amine-based polyether has the following structural formula:
Because the interference components in the drilling fluid are constantly changing, the interference cannot be eliminated by directly subtracting a blank titration method, and therefore the drilling fluid filtrate needs to be treated.
Firstly, preparing amino polyether standard solutions with different concentrations, mixing and stirring the amino polyether standard solutions with different concentrations and an alcohol solvent, standing and filtering to obtain filtrate;
wherein the concentrations of the amino polyether standard solutions with different concentrations are 0g/L, 10g/L, 20g/L and 30 g/L.
The alcohol solvent added into the standard solution in the steps utilizes the special hydrophily and lipophilicity of the alcohol solvent, so that the amino polyether in the filtrate can be completely dissolved, the inorganic treating agent and the macromolecular treating agent which can interfere with the measurement in the filtrate are not dissolved, and the interference of the colored treating agent in the filtrate can be eliminated.
In the present invention, the alcohol solvent is selected from ethanol, isopropanol or propanol, preferably isopropanol.
The volume ratio of the alcohol solvent to the amino polyether standard solution is greater than 7:3, when the volume ratio of the alcohol solvent to the amino polyether standard solution is greater than 7:3, the hydroxide radical and the amino radical can be titrated step by using a double indicator, and meanwhile, the interference of other treating agents is fully eliminated, in some specific embodiments of the invention, the volume ratio of the alcohol solvent to the amino polyether standard solution is (7-9): (1-3), in other embodiments of the present invention, the volume ratio of the alcohol solvent to the amine-based polyether standard solution is 9: 1.
The standing time is 20-40 min, preferably 30-35 min, the standing temperature is normal temperature, and in the invention, the normal temperature is defined as 25 +/-5 ℃.
After the filtrate was obtained, titration was performed stepwise using double indicators. Specifically, 40-60 ml of the filtrate is taken, the filtrate is required to be accurately measured, and the same amount is required when a standard curve is drawn and the liquid to be measured is measured. Adding 2 drops of phenolphthalein indicator with mass concentration of 1%, titrating with hydrochloric acid-alcohol solvent solution until colorless, then adding 5 drops of bromophenol blue indicator with mass concentration of 2%, titrating with hydrochloric acid-alcohol solvent solution until the color turns yellow from blue.
In the present invention, since the titration to colorless process does not require recording the amount of the hydrochloric acid consumed, the concentration of the hydrochloric acid-alcohol solvent solution is not particularly limited in the present invention, and preferably, the same hydrochloric acid solution can be used for the two-step titration.
In some embodiments of the invention, the concentration of the hydrochloric acid-alcohol solvent solution used in the titration to colorless process is 0.08-0.14 mol/L, preferably 0.10-0.12 mol/L; the concentration of the hydrochloric acid-alcohol solvent solution used in the process of titration until the blue color turns yellow is 0.08-0.14 mol/L, and preferably 0.10-0.12 mol/L.
The alcohol solvent is selected from ethanol, isopropanol or propanol, preferably isopropanol.
Recording the volume of the hydrochloric acid-alcohol solvent solution consumed in the process from blue to yellow, calculating the amount of the substance consuming the hydrochloric acid according to the concentration of the hydrochloric acid-alcohol solvent solution, and drawing a linear relation standard curve of the concentration of the amine polyether and the amount of the substance consuming the hydrochloric acid.
And after a standard curve is obtained, determining the content of the amino polyether in the filtrate of the drilling fluid to be detected.
Mixing and stirring the filtrate of the drilling fluid to be tested and an alcohol solvent, standing and filtering to obtain a filtrate.
And the drilling fluid filtrate to be measured is the drilling fluid filtrate in which the content of the amino polyether is to be measured. The drilling fluid is a water-based drilling fluid comprising: polymer drilling fluid, polysulfonate drilling fluid, saturated brine drilling fluid, potassium chloride drilling fluid, polymer potassium chloride drilling fluid and amino polyether drilling fluid.
The alcohol solvent is selected from ethanol, isopropanol or propanol, preferably isopropanol.
In the invention, the alcohol solvent used for drawing the standard curve is the same as the alcohol solvent used for measuring the content of the amino polyether in the filtrate of the drilling fluid to be measured.
The volume ratio of the alcohol solvent to the filtrate of the drilling fluid to be detected is greater than 7:3, when the volume ratio of the alcohol solvent to the filtrate of the drilling fluid to be detected is greater than 7:3, the hydroxide radical and the amino radical can be titrated step by using double indicators, and meanwhile, the interference of other treating agents is considered to be fully eliminated, in some specific embodiments of the invention, the volume ratio of the alcohol solvent to the filtrate of the drilling fluid to be detected is (7-9): (1-3), in other specific embodiments of the present invention, the volume ratio of the alcohol solvent to the drilling fluid filtrate to be tested is 9: 1.
The standing time is 20-40 min, preferably 30-35 min, the standing temperature is normal temperature, and in the invention, the normal temperature is defined as 25 +/-5 ℃.
After the filtrate was obtained, titration was performed stepwise using double indicators. Specifically, 50ml of the filtrate is added with 2 drops of a phenolphthalein indicator with the mass concentration of 1%, and is titrated to be colorless by using a hydrochloric acid-alcohol solvent solution, then 5 drops of a bromophenol blue indicator are added, and is titrated to be changed from blue to yellow by using a hydrochloric acid-alcohol solvent solution.
In the process from titration to colorless, the concentration of the hydrochloric acid-alcohol solvent solution is not particularly limited because the amount of the consumed hydrochloric acid does not need to be recorded, and preferably, the same hydrochloric acid solution can be directly used for the two-step titration.
In some embodiments of the invention, the concentration of the hydrochloric acid-alcohol solvent solution used in the titration to colorless process is 0.08-0.14 mol/L, preferably 0.10-0.12 mol/L; the concentration of the hydrochloric acid-alcohol solvent solution used in the process of titration until the blue color turns yellow is 0.08-0.14 mol/L, and preferably 0.10-0.12 mol/L.
In the hydrochloric acid-alcohol solvent solution, the alcohol solvent is selected from ethanol, isopropanol or propanol, preferably isopropanol.
Preferably, in the present invention, the concentrations of the hydrochloric acid-alcohol solvent solutions used in the respective steps are the same.
Recording the volume of the hydrochloric acid-alcohol solvent solution consumed in the process from blue to yellow, calculating the amount of hydrochloric acid consumed by the filtrate according to the concentration of the hydrochloric acid-alcohol solvent solution, and obtaining the content of the amino polyether in the filtrate of the drilling fluid according to the obtained linear relation standard curve.
In the invention, when a standard curve is drawn and the content of the amino polyether in the filtrate of the drilling fluid to be measured is measured, double indicators, namely a phenolphthalein indicator and a bromophenol blue indicator, are adopted to titrate hydroxyl and amino step by step, thereby eliminating the interference of free hydroxyl. The hydroxyl and the amino in the pure water solvent turn red when meeting phenolphthalein, but the polarity of the solvent is gradually reduced along with the gradual increase of the proportion of the alcohols, and the amino does not turn red when meeting phenolphthalein and the hydroxyl can still turn red.
The invention adopts a conventional titration analysis method, does not need special instruments and equipment, is simple, convenient and quick, and is suitable for drilling site monitoring. The invention adopts a method of adding an alcohol solvent into the filtrate of the drilling fluid for treatment, thereby eliminating the interference of an inorganic treating agent and a macromolecular treating agent in the filtrate and simultaneously eliminating the interference of the color of the filtrate; hydroxyl and amino are respectively titrated by adopting a method of double indicator titration of a phenolphthalein indicator and a bromophenol blue indicator, so that the interference of free hydroxyl is eliminated, and the content of amino polyether in the filtrate of the drilling fluid is determined. The recovery rate of the added standard is more than 92%, and the relative standard deviation is less than 5%, which indicates that the monitoring method is feasible and has better reproducibility. The problem that the content of the amino polyether is difficult to directly measure due to the complex components of the drilling fluid filtrate and a plurality of interference factors is solved. The method fills the gap of monitoring the content of the amino polyether in the filtrate of the drilling fluid, can timely master the change condition of the effective content of the amino polyether in the drilling fluid on site, is beneficial to timely maintenance and supplement of drilling fluid engineers on site, and has important significance for guiding site construction.
For further understanding of the present invention, the method for monitoring the content of amine-based polyether in drilling fluid filtrate in situ provided by the present invention is described below with reference to the following examples, and the scope of the present invention is not limited by the following examples.
Example 1
And (3) measuring the free content of the amino polyether in the drilling fluid of different well depths of a certain 1 well.
The well uses a polymer drilling fluid, and the drilling fluid basic formula comprises the following components: 4% of prehydrated bentonite slurry, 0.7% of hydrolyzed polyacrylonitrile ammonium salt, 0.3% of polyacrylamide, 0.3% of low-viscosity emulsion polymer, 0.3% of high-viscosity emulsion polymer, 2% of superfine calcium carbonate, 1% of oil-soluble temporary plugging agent, 0.7% of emulsifier, 4% of crude oil, 2% of amino polyether I and the balance of water, wherein the concentrations in the formula are mass concentrations which are the same as the following. The amino polyether I has a number average molecular weight of about 230 and has the following structural formula:
the monitoring steps are as follows:
step 1: drawing a standard curve:
before the amino polyether is added into the well, taking blank drilling fluid filtrate, dividing into 4 parts, each 10mL, accurately adding 0g, 0.1g, 0.2g and 0.3g (accurate to 0.0001g) of amino polyether respectively to obtain amino polyether standard solutions with the concentrations of 0g/L, 10g/L, 20g/L and 30g/L respectively, then adding 90mL of isopropanol into each standard solution respectively, stirring for 1min, fully mixing, sealing and standing at room temperature for 30min, filtering by using a common funnel, collecting filtrate, taking 50mL of filtrate, adding 2 drops of phenol phthalein indicator with the mass concentration of 1%, titrating to be colorless by using 0.10mol/L hydrochloric acid-isopropanol standard solution, then adding 5 drops of 2% bromophenol blue indicator, titrating to be yellow from blue by using 0.10mol/L hydrochloric acid-isopropanol standard solution, recording the volume of hydrochloric acid consumed in the process from blue to yellow, the amount of the substance consuming hydrochloric acid was calculated from the hydrochloric acid concentration, and a standard curve of the linear relationship between the amine-based polyether concentration and the hydrochloric acid consumption was plotted, and the result is shown in FIG. 1.
Step 2: taking 8mL of drilling fluid filtrate to be measured, adding isopropanol according to the volume ratio of the alcohol solvent to the drilling fluid filtrate of 9:1, stirring for 1min, fully and uniformly mixing, standing at room temperature in a closed manner for 30min, filtering by using a common funnel, and collecting filtrate.
And step 3: 50mL of the filtrate was taken, 2 drops of phenolphthalein indicator with a mass concentration of 1% were added, the mixture was titrated with 0.10mol/L hydrochloric acid-isopropanol standard solution until colorless, 5 drops of bromophenol blue indicator were added, the mixture was titrated with 0.10mol/L hydrochloric acid-isopropanol standard solution until the color changed from blue to yellow, and the volume of hydrochloric acid consumed from blue to yellow was recorded.
And 4, step 4: and (3) calculating the amount of the hydrochloric acid consumed substance of the liquid to be detected according to the volume and concentration of the hydrochloric acid consumed in the step (3), and obtaining the content of the amino polyether in the filtrate of the drilling fluid by contrasting a linear relation standard curve of the concentration of the amino polyether and the hydrochloric acid consumed, wherein the result is shown in the following table 1.
TABLE 1 amine-based polyether content in drilling fluid filtrate from a 1-well
As can be seen from Table 1, as the well depth increases, the amine-based polyether consumption gradually increases and the free content gradually decreases, which should be replenished at the appropriate time.
Example 2
And (3) measuring the content of the amino polyether in the filtrate of the drilling fluid of a certain 2 wells. The second well is drilled in the presence of 23 salts, and a brine drilling fluid is used for drilling, wherein the basic formula of the drilling fluid is as follows: 4% of prehydrated bentonite slurry, 0.5% of hydrolyzed polyacrylonitrile ammonium salt, 0.3% of polyacrylamide, 0.5% of low-viscosity polyanionic cellulose, 0.3% of low-viscosity emulsion polymer, 2% of superfine calcium carbonate, 2% of asphalt powder, 0.2% of chemical cleaning agent, 0.8% of sodium hydroxide, 25% of sodium chloride and 1% of amine polyether II, the balance of water, wherein the amine polyether II is a poly (propylene oxide) compound terminated by primary amino, contains three primary amino groups, has the number average molecular weight of about 440, and has the following structural formula:
the monitoring steps are as follows:
(1) drawing a standard curve
The method is the same as example 1, except that the hydrochloric acid-isopropanol standard solution is changed into hydrochloric acid-propanol standard solution, the concentration is changed into 0.14mol/L, and the obtained amino polyether is concentratedThe linear relation standard curve of degree and hydrochloric acid consumption is shown in fig. 2, the fitted linear regression equation is that y is 0.0326x +0.0703, and the correlation coefficient R20.998, wherein x represents the free content of amine-based polyether in g/L and y represents the amount of hydrochloric acid consumed in mmol.
(2) Taking 6mL of drilling fluid filtrate to be measured, adding propanol according to the volume ratio of the alcohol solvent to the drilling fluid filtrate of 9:1, stirring for 1min, fully and uniformly mixing, standing at room temperature in a closed manner for 20min, filtering by using a common funnel, and collecting filtrate.
(3) 50mL of the filtrate was taken, 2 drops of phenolphthalein indicator with a mass concentration of 1% were added, the mixture was titrated with 0.14mol/L hydrochloric acid-propanol standard solution until colorless, 5 drops of bromophenol blue indicator were added, the mixture was titrated with 0.14mol/L hydrochloric acid-propanol standard solution until the color changed from blue to yellow, and the volume of hydrochloric acid consumed from blue to yellow was recorded.
(4) And (4) calculating the amount of the hydrochloric acid consumed by the liquid to be detected according to the volume and the concentration of the hydrochloric acid consumed in the step (3), and obtaining the content of the amino polyether in the filtrate of the drilling fluid by contrasting a linear relation standard curve of the concentration of the amino polyether and the hydrochloric acid consumed, wherein the result is shown in the following table 2.
TABLE 2 amine-based polyether content in 2-well drilling fluid filtrate
As can be seen from Table 2, when the amount of the amino polyether added in the formulation is 1%, i.e., the content is 10g/L, the free content of the amino polyether is reduced to 6.4g/L along with the loss in the drilling process, and the amino polyether should be properly supplemented.
Example 3
And (3) measuring the content of the amino polyether in the filtrate of the drilling fluid of a certain 3 wells. The well three-opening is drilled by using polysulfonate drilling fluid, and the basic formula of the drilling fluid is as follows: 4% of prehydrated bentonite slurry, 0.4% of polymer fluid loss additive, 0.3% of low-sodium carboxymethylcellulose, 2% of sulfonated phenolic resin, 2% of sulfonated lignite, 0.12% of NaOH, 2.5% of aminopolyether III and the balance of water, wherein the aminopolyether III has a number average molecular weight of about 600 and has the following structural formula:
The monitoring steps are as follows:
(1) drawing a standard curve
The method is the same as example 1, except that the hydrochloric acid-isopropanol standard solution is changed into hydrochloric acid-ethanol standard solution, the concentration is changed to 0.08mol/L, the obtained standard curve of the linear relation between the concentration of the amino polyether and the consumed hydrochloric acid is shown in figure 3, the fitted linear regression equation is that y is 0.0164x +0.0538, and the correlation coefficient R is20.9989, where x represents the free amine polyether content in g/L and y represents the amount of hydrochloric acid consumed in mmol.
(2) Taking 10mL of drilling fluid filtrate to be tested, adding ethanol according to the volume ratio of the alcohol solvent to the drilling fluid filtrate of 9:1, stirring for 1min, fully and uniformly mixing, standing at room temperature in a closed manner for 40min, filtering by using a common funnel, and collecting filtrate.
(3) Taking 50mL of the filtrate, adding 2 drops of phenolphthalein indicator with the mass concentration of 1%, titrating with 0.08mol/L hydrochloric acid-ethanol standard solution until the filtrate is colorless, adding 5 drops of 2% bromophenol blue indicator, titrating with 0.08mol/L hydrochloric acid-ethanol standard solution until the filtrate is changed from blue to yellow, and recording the volume of the consumed hydrochloric acid in the process from blue to yellow.
(4) And (4) calculating the amount of the hydrochloric acid consumed by the liquid to be detected according to the volume and concentration of the hydrochloric acid consumed in the step (3), and obtaining the content of the amino polyether in the filtrate of the drilling fluid by contrasting a linear relation standard curve of the concentration of the amino polyether and the hydrochloric acid consumed, wherein the result is shown in the following table 3.
TABLE 3 Aminopolyether content in 3-well drilling fluid filtrate
Example 4 verification of the accuracy of the method
A water-based drilling fluid system is prepared indoors, and the basic formula of the system is as follows: the method comprises the following steps of (1) adding water, 0.4% of macromolecular polyacrylamide, 0.5% of low-sodium carboxymethyl cellulose, 0.3% of hydrolyzed polyacrylonitrile ammonium salt, 0.5% of carboxymethyl starch, 1% of polyalcohol and 0.1% of sodium hydroxide, (bentonite is not added in the formula because the bentonite can adsorb amine polyether if being added, and the adsorption quantity is unknown, the theoretical content of the amine polyether in the filtrate of the drilling fluid can not be determined, the accuracy of the method can not be verified, and therefore, the bentonite is not added).
Since the components of the drilling fluid used in the field are constantly changed, in order to simulate the field as much as possible, the drilling fluid is divided into three groups, which respectively represent the drilling fluid of the same well at different periods. The first group is regarded as new well-matched drilling fluid (at the moment, the amino polyether is not added, and can be used as blank filtrate); and the second group is aged for 48 hours at 120 ℃ in a rolling way, then 3 percent of potassium chloride, 1.0 percent of calcium chloride and 0.2 percent of sodium hydroxide are added, the drilling fluid is considered as the drilling fluid after the formula is adjusted in the field maintenance process, and then amino polyether I with different known amounts is added (here, if the amino polyether is added and then aged in a rolling way, the theoretical content of the amino polyether in the filtrate of the drilling fluid cannot be determined due to the degradation of the amino polyether, and the accuracy of the method cannot be verified, so the amino polyether is added after the aging is selected in the experiment). And the third group is formed by adding 2% of sulfonated phenolic resin and 2% of sulfonated lignite on the basis of the second group, and is regarded as the drilling fluid added with the high-temperature resistant fluid loss additive along with the increase of the well depth. Using the second and third groups of drilling fluid filtrates as the to-be-detected fluids, determining the content of the amino polyether in the filtrate by the method described in example 1, (drawing a standard curve for the same well, wherein the blank filtrate used in drawing the standard curve is the drilling fluid filtrate without the amino polyether in the first group), and drawing to obtain a standard curve equation: y 0.0421x + 0.0514. The results of measuring the free content of the amine-based polyether are shown in tables 4 and 5 below. The result shows that the determination error is less than 5%, and the requirement of on-site monitoring can be met.
TABLE 4 method accuracy verification in Water-based drilling fluids (second group of drilling fluids)
TABLE 5 method accuracy verification in Water-based drilling fluids (third group of drilling fluids)
Comparative example 1
This comparative example is the direct titration of the aminopolyether content of the second and third drilling fluid filtrates from example 4 with a hydrochloric acid-isopropanol standard solution. The specific operation steps are as follows:
(1) drawing a standard curve
Dividing the blank drilling fluid filtrate into 4 parts, each part is 5mL, accurately adding 0g, 0.05g, 0.1g and 0.15g (to the accuracy of 0.0001g) of amino polyether respectively, to obtain the amino polyether standard solutions with the concentrations of 0g/L, 10g/L, 20g/L and 30g/L respectively, adding water according to the volume ratio of 9:1 of water to the amino polyether standard solution, adding 2 drops of phenolphthalein indicator with the mass concentration of 1%, titrating with 0.10mol/L hydrochloric acid-isopropanol standard solution until the solution is colorless, then adding 5 drops of bromophenol blue indicator with mass concentration of 2%, titrating with 0.10mol/L hydrochloric acid-isopropanol standard solution until the color turns yellow from blue, recording the volume of the consumed hydrochloric acid in the process from blue to yellow, and calculating the amount of the substances consuming the hydrochloric acid according to the concentration of the hydrochloric acid, and drawing a linear relation standard curve of the concentration of the amine polyether and the consumed hydrochloric acid. The standard curve equation obtained by drawing is as follows: y is 0.0419x +0.0014
(2) Titration of the test solution
Dissolving 5mL of drilling fluid filtrate to be tested in 45mL of water, adding 5 drops of a bromophenol blue indicator of 2g/L, titrating with a hydrochloric acid-isopropanol standard solution of 0.10mol/L, and recording the volume of hydrochloric acid consumed in the process of changing blue into yellow.
(3) Computing
And calculating the amount of the substance consuming the hydrochloric acid according to the concentration and the volume of the hydrochloric acid, and substituting the amount into a linear relation standard curve of the concentration of the amino polyether and the consumed hydrochloric acid to obtain the concentration of the amino polyether.
The results of the second set of drilling fluid filtrates from example 4, as measured by the method of this comparative example, are shown in table 6. The results show that when the content of the amino polyether in the filtrate of the drilling fluid is measured by directly titrating the hydrochloric acid-isopropanol standard solution, the error is large, and the requirement of on-site monitoring cannot be met. Although the blank filtrate is adopted to draw a standard curve in the comparative example, the measurement error is reduced to a certain extent, the treatment agent is degraded after rolling aging, the components capable of reacting with hydrochloric acid are increased, and the formula of the drilling fluid is adjusted, so that the measurement result is increased. During on-site real drilling, the drilling fluid is in a continuous cyclic aging state, and meanwhile, due to the reasons of solid phase adsorption, formula adjustment and the like, the components of the drilling fluid are always in a changing state, so that the content of the amino polyether cannot be directly monitored by adopting a hydrochloric acid-isopropanol standard solution titration method.
When the filtrate of the third group of drilling fluid in example 4 is measured by the method of the comparative example, the endpoint cannot be judged due to the fact that the filtrate is dark in color (both the high-temperature-resistant filtrate reducer sulfonated phenolic resin and the sulfonated lignite are colored treatment agents).
TABLE 6 direct determination of the aminopolyether content in the drilling fluid filtrate
Comparative example 2
This comparative example titrates the amine-based polyether content of the third drilling fluid set described in example 4 using the bromophenol blue indicator alone without the dual indicator. The procedure is as in example 4 except that in this comparative example, no phenolphthalein indicator is added, and 5 drops of 2% bromophenol blue indicator are added directly. The titration end point is obvious in color change, and the drawn standard curve equation is as follows: y is 0.0423x +0.1614, and the amine-based polyether content of the drilling fluid filtrate is measured and is shown in table 7 below.
As can be seen from Table 7, the measurement error is large and the on-site monitoring requirement cannot be met. This is because the interference of hydroxide in the filtrate cannot be completely eliminated by using bromophenol blue indicator alone without using phenolphthalein indicator, resulting in a high measurement result.
TABLE 7 determination of the amine polyether content in drilling fluid filtrate without dual indicators
Comparative example 3
This comparative example was conducted without the use of alcoholic solvents to directly determine the amine-based polyether content of the second and third drilling fluid filtrates described in example 4. The procedure was as in example 4 except that the isopropanol used in the treatment of the drilling fluid filtrate was replaced by water. In the experimental process, the hydrochloric acid consumed by the process of changing the color from red to colorless by adding the phenolphthalein indicator is obviously increased, because in the aqueous solution, the phenolphthalein can be changed into red by hydroxyl and amino in amino polyether, the hydrochloric acid consumed by the corresponding process of adding the bromophenol blue indicator from blue titration to the end point is obviously reduced, and the color change of the titration end point is not as obvious as that in an alcohol solvent. The results of measuring the content of the aminopolyethers in the second group of drilling fluid filtrate are shown in the following table 8, and the results show that the measurement deviation is large and the field requirement cannot be met.
When the filtrate of the third group of drilling fluid in example 4 is measured by the method of the present comparative example, the endpoint cannot be finally determined due to the darker color of the filtrate.
TABLE 8 determination of the aminopolyether content in drilling fluid filtrate without the use of alcohol solvents
Example 5 verification of the accuracy of the method in different drilling fluid systems
Preparing a common drilling fluid system indoors: polymer, polysulfonate, saturated brine, polymer potassium chloride drilling fluid, system formulation is shown in table 9 below. After the prepared drilling fluid is aged for 16 hours at 120 ℃, 2 percent of amino polyether I is added, namely, the content of the amino polyether is 20 g/L. The content of the amino polyether in the filtrate is determined according to the method in the embodiment 1, the result is shown in the following table 10, and as can be seen from the result, the determination error is less than 5%, the on-site monitoring requirement can be met, and the determination method is suitable for monitoring the content of the amino polyether in the filtrate of the on-site common drilling fluid.
TABLE 9 drilling fluid system formulation
TABLE 10 method accuracy verification in drilling fluids
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A field monitoring method for the content of amino polyether in drilling fluid filtrate is characterized by comprising the following steps:
A) drawing a standard curve:
taking a plurality of parts of blank drilling fluid filtrate, and adding amino polyether with different mass to obtain amino polyether standard solutions with different concentrations, wherein the blank drilling fluid filtrate is drilling fluid filtrate without amino polyether;
respectively mixing and stirring the amino polyether standard solutions with different concentrations and an alcohol solvent, standing and filtering to obtain filtrate;
taking the filtrate, adding a phenolphthalein indicator, titrating the filtrate to be colorless by using a hydrochloric acid-alcohol solvent solution, then adding a bromophenol blue indicator, titrating the filtrate by using a hydrochloric acid-alcohol solvent solution until the filtrate turns yellow from blue, recording the volume of the hydrochloric acid-alcohol solvent solution consumed in the process from blue to yellow, calculating the amount of substances consuming hydrochloric acid according to the concentration of the hydrochloric acid-alcohol solvent solution, and drawing a linear relation standard curve of the concentration of the amino polyether and the amount of the substances consuming hydrochloric acid;
B) and (3) determining the content of the amino polyether in the filtrate of the drilling fluid to be detected:
mixing and stirring the filtrate of the drilling fluid to be detected and an alcohol solvent, standing and filtering to obtain filtrate;
and taking the filtrate, adding a phenolphthalein indicator, titrating with a hydrochloric acid-alcohol solvent solution until the filtrate is colorless, adding a bromophenol blue indicator, titrating with a hydrochloric acid-alcohol solvent solution until the filtrate turns yellow from blue, recording the volume of the hydrochloric acid-alcohol solvent solution consumed in the process from blue to yellow, calculating the amount of hydrochloric acid consumed by the filtrate according to the concentration of the hydrochloric acid-alcohol solvent solution, and calculating the content of the amino polyether in the filtrate of the drilling fluid according to the linear relation standard curve obtained in the step A).
2. The method of claim 1, wherein the drilling fluid is a water-based drilling fluid comprising: polymer drilling fluid, polysulfonate drilling fluid, saturated brine drilling fluid, potassium chloride drilling fluid, polymer potassium chloride drilling fluid and amino polyether drilling fluid.
3. The method according to claim 1, wherein the amine-based polyether standard solutions with different concentrations have concentrations of 0g/L, 10g/L, 20g/L and 30 g/L.
4. The method of claim 1, wherein the phenolphthalein indicator is present at a concentration of 1% by mass and the bromophenol blue indicator is present at a concentration of 2% by mass.
5. The method according to claim 1, wherein the alcoholic solvent in step a) and the alcoholic solvent in step B) are the same alcoholic solvent, and the alcoholic solvent is selected from ethanol, isopropanol or propanol.
6. The method as claimed in claim 1, wherein in step a), the volume ratio of the alcohol solvent to the amine-based polyether standard solution is greater than 7: 3;
in the step B), the volume ratio of the alcohol solvent to the filtrate of the drilling fluid to be detected is more than 7: 3;
the volume ratio of the alcohol solvent to the amino polyether standard solution is the same as the volume ratio of the alcohol solvent to the drilling fluid filtrate to be measured.
7. The method according to claim 1, wherein in step A), the concentration of the hydrochloric acid-alcohol solvent solution used in the titration to colorless process is 0.08-0.14 mol/L; the concentration of a hydrochloric acid-alcohol solvent solution used in the process of titrating until the blue color turns yellow is 0.08-0.14 mol/L;
in the step B), the concentration of a hydrochloric acid-alcohol solvent solution used in the process of titration to colorless is 0.08-0.14 mol/L; the concentration of the hydrochloric acid-alcohol solvent solution used in the process of titrating until the blue color turns yellow is 0.08-0.14 mol/L.
8. The method according to claim 1, wherein in the step A), the standing time is 20-40 min, and the temperature is 25 +/-5 ℃;
in the step B), the standing time is 20-40 min, and the temperature is 25 +/-5 ℃.
9. The method of claim 1, wherein the amine-based polyether has a polyether structure as a main chain, and the terminal reactive functional group comprises a polymer containing amine groups, and has a number average molecular weight of less than 1000.
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