CN104458620A - Method for detecting concentration of polymer for oil displacement - Google Patents
Method for detecting concentration of polymer for oil displacement Download PDFInfo
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- CN104458620A CN104458620A CN201410775942.7A CN201410775942A CN104458620A CN 104458620 A CN104458620 A CN 104458620A CN 201410775942 A CN201410775942 A CN 201410775942A CN 104458620 A CN104458620 A CN 104458620A
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Abstract
The invention discloses a method for detecting concentration of a polymer for oil displacement. The method comprises the following steps: (1) preparing the standard aqueous solutions of the polymer of at least five different concentrations; (2) respectively adding a digesting agent and aids into the standard aqueous solutions of the polymer, heating to carry out a digestion reaction, cooling, adding an acid solution, and respectively measuring the absorbance of the digested standard aqueous solutions of the polymer and the reference at the wavelengths of 220nm and 275nm by utilizing an ultraviolet spectrophotometer; respectively calculating the corrected absorbance of the standard aqueous solutions of the polymer and the reference, and drawing a standard curve by taking the concentration of the standard aqueous solutions of the polymer as a horizontal coordinate, and taking the difference of the corrected absorbance of the standard aqueous solutions of the polymer and the corrected absorbance of the reference solution as a vertical coordinate; (3) taking a to-be-measured polymer sample for oil displacement, and repeating the step (2), thereby obtaining the concentration of the polymer. The method disclosed by the invention is easy and rapid to operate, batch detection can be realized, the cost is reduced, the precision and accuracy are high, the equipment is small and portable, and the method has on-site oilfield application prospects.
Description
Technical field
The present invention relates to a kind of detection method of Polymer Used For Oil Displacement concentration, be specifically related to a kind of detection method of polyacrylamide polymers for oil displacement polymer concentration.
Background technology
Polymer displacement of reservoir oil tech, as one of dominant technology improving oil recovery factor, is widely applied in oil fields such as China's grand celebration, triumph, huge port, Henan, the Bohai Sea, creates good economic benefit.Partially hydrolyzed polyacrylamide is the oil displacement agent be most widely used in polymer displacement of reservoir oil tech.It is an important content of polymer flooding dynamic monitoring that polymer concentration accurately detects, to guarantee polymer injection allocation effect, tracking in time polymer flooding dynamically, adjustment is poly-drives scheme and carry out poly-numerical simulation of driving significant, being that impact is poly-drives one of key factor of field test and industrialization successful implementation.At present, the CdI_2-starch method of Oil Field widespread use, complex operation step, requires high to the making of typical curve, the bromine water used and glacial acetic acid, and tool severe corrosive and volatility all exist harm to the healthy of testing staff and environment.
Summary of the invention
The object of this invention is to provide a kind of detection method of Polymer Used For Oil Displacement concentration, by measuring the nitrogen in polymkeric substance, realize the detection to polymer concentration, the method is simple and quick, and equipment is simple, convenient to operation, the nontoxic difficulty volatilization of agents useful for same, environmentally safe, data reappearance is good, precision and accuracy high.
The detection method of Polymer Used For Oil Displacement concentration provided by the invention, comprises the steps:
(1) adopt on-the-spot injection allocation water, prepare the Polymer Standards aqueous solution of at least 5 variable concentrations respectively;
(2) in described Polymer Standards aqueous solution, add digestion agent and auxiliary agent respectively, and heating is carried out clearing up reaction, adds acid solution after cooling; Utilize ultraviolet spectrophotometer, measure the absorbance of the Polymer Standards solution after clearing up at wavelength 220nm and 275nm place respectively, be designated as (A respectively
x)
220(A
x)
275, the X in formula is the label of described Polymer Standards solution, and X is natural number; Measure the absorbance of reference at wavelength 220nm and 275nm place respectively, be designated as (A respectively
0)
220(A
0)
275;
Described reference is described on-the-spot injection allocation water;
(1) and (2) calculates the correction absorbance of described Polymer Standards aqueous solution and described reference respectively according to the following equation, is designated as A respectively
xand A
0,
A
X＝(A
X)
220－2(A
X)
275(1)
A
0＝(A
0)
220－2(A
0)
275(2)
(3) calculate the difference of the correction absorbance of described Polymer Standards aqueous solution and the correction absorbance of described reference according to the following equation, are designated as A,
A＝A
x－A
o(3)
With the concentration of described Polymer Standards aqueous solution for horizontal ordinate, the difference A of the correction absorbance of described Polymer Standards aqueous solution and the correction absorbance of described reference solution is ordinate, drawing standard curve linear equation;
(3) get Polymer Used For Oil Displacement sample to be measured, repeat above-mentioned steps (2), obtain the difference of the correction absorbance of Polymer Used For Oil Displacement sample to be measured and the correction absorbance of described reference; Namely the concentration of described Polymer Used For Oil Displacement sample to be measured is obtained according to described linear equation.
In above-mentioned detection method, described polymkeric substance is polyacrylamide.
In above-mentioned detection method, the molecular weight of described polyacrylamide is 800 ~ 2,800 ten thousand, specifically can be 1,200 ten thousand ~ 2,000 ten thousand, 1,200 ten thousand ~ 1,800 ten thousand, 1,800 ten thousand ~ 2,000 ten thousand, 1,200 ten thousand, 1,800 ten thousand or 2,000 ten thousand; Degree of hydrolysis is 10% ~ 50%, specifically can be 35% ~ 46%, 35% ~ 40%, 40% ~ 46%, 35%, 40%, 46% etc.
In above-mentioned detection method, the concentration of described Polymer Standards aqueous solution is 0 ~ 300mg/L, specifically can be 0,20,40,60,80,100,120,140,160,180,200,220,240,260,280 and 300mg/L.
In above-mentioned detection method, described Polymer Standards aqueous solution can be diluted by polymer mother liquor and be obtained; Described polymer mother liquor obtains through hold over night after being mixed with described on-the-spot injection allocation water by Polymer Standards product, specifically obtain through stirring by being joined at Oil Field injection allocation temperature by Polymer Standards product (polymer dry powder) in on-the-spot injection allocation water, described stirring rate can be 300 ~ 500rpm;
The concentration of described polymer mother liquor can be 5000 ~ 10000mg/L, specifically can be 5000mg/L.
In above-mentioned detection method, described digestion agent is potassium persulfate, and described auxiliary agent is sodium hydroxide solution;
The addition of described digestion agent and described auxiliary agent is as follows: after described in 1mL, Polymer Standards aqueous solution is diluted with water to 10mL, and the addition of described digestion agent is 0.5g, and the addition of described auxiliary agent is 1mL, and the concentration of described auxiliary agent is 0.5g/L.
In above-mentioned detection method, described in clear up reaction temperature be 120 ~ 124 DEG C, specifically can be 120 DEG C; The described time of clearing up reaction is 30 ~ 50min, specifically can be 30min;
Described cooling is down to 20 ~ 30 DEG C, and described cooling fully mixes afterwards.
In above-mentioned detection method, described acid solution is hydrochloric acid solution;
The addition of described acid solution is as follows: after described in 1mL, Polymer Standards aqueous solution is diluted with water to 10mL, and the addition of described acid solution is 1mL, and the concentration of described acid is 0.2g/L.
In above-mentioned detection method, after adding acid solution, also comprise the step of natural subsidence, settling time more than 30min, get supernatant and measure.
In above-mentioned detection method, if the concentration of polymkeric substance is more than 300mg/L in described Polymer Used For Oil Displacement sample to be measured, by diluting concentration adjustment in the range of linearity, specifically 2 ~ 10 times can be diluted.
The detection method of Polymer Used For Oil Displacement concentration provided by the invention, the nontoxic difficulty volatilization of agents useful for same, simple and efficient to handle, can realize batch detection (25-30/person-time, 2h), cost reduces precision and accuracy high (error is all less than 3%), equipment is little portable, have Oil Field application prospect, the polymkeric substance that especially can realize the inclement condition places such as offshore platform, desert, Gobi desert detects fast.
Accompanying drawing explanation
Fig. 1 is the typical curve of polyacrylamide in embodiment 1 (degree of hydrolysis is 35%, and molecular weight is 1,200 ten thousand).
Fig. 2 is the typical curve of polyacrylamide in embodiment 2 (degree of hydrolysis is 40%, and molecular weight is 1,200 ten thousand).
Fig. 3 is the typical curve of polyacrylamide in embodiment 3 (degree of hydrolysis is 46%, and molecular weight is 1,200 ten thousand).
Embodiment
The experimental technique used in following embodiment if no special instructions, is conventional method.
Material used in following embodiment, reagent etc., if no special instructions, all can obtain from commercial channels.
The detection of embodiment 1, Polyacrylamides For Enhanced Oil Recoveries concentration
The degree of hydrolysis adopted certain Oil Field is 35%, and molecular weight is that the concentration of 1,200 ten thousand polyacrylamide solutions detects, and step is as follows:
1) 50 DEG C, above-mentioned polyacrylamide dry powder is mixed with on-the-spot injection allocation water under 400rpm condition, hold over night after dissolving completely, obtains 5000mg/L polyacrylamide mother liquor.Through polymer mother liquor with on-the-spot injection allocation water be diluted to concentration be respectively 0,20,40,60,80,100,120,140,160,180,200,220,240,260,280, the polyacrylamide standard aqueous solution of 300mg/L.
2) the above-mentioned polyacrylamide standard aqueous solution of 1mL is pipetted respectively in color comparison tube, be diluted with water to 10mL, add 0.5g potassium persulfate powder, 1mL NaOH solution (0.5g/L), shakes up, color comparison tube is placed in WTWCR2200 type heating and decompose device, continue to be heated to 120 DEG C and start timing, after insulation 30min, remove enclosing cover, take out color comparison tube and be cooled to 25 DEG C, acutely rock 10min.Mix after adding the HCl solution (0.2g/L) of 1mL in color comparison tube, after leaving standstill natural subsidence 30min, get supernatant.Use quartz colorimetric utensil, on ultraviolet spectrophotometer, make reference with on-the-spot injection allocation water, measure absorbance respectively at wavelength 220nm and 275nm place.The absorbance of zero-dose is designated as A
0, other concentration absorbance be designated as A
x, correct absorbance A according to following formulae discovery:
A
0＝(A
0)
220－2(A
0)
275
A
X＝(A
X)
220－2(A
X)
275
A＝A
X－A
0。
With polymkeric substance (polyacrylamide) concentration (C, mg/L) for horizontal ordinate, corresponding A value is ordinate, draws A-C typical curve (Fig. 1), matching A-C linear relationship equation: A=0.00133 × C+0.01867.
3) compound concentration be 30,50,70,90,110,130,150,170,190,210,230,250,270, the polyacrylamide solution of 290mg/L, repeat 2) step, bring the A value of gained into A-C linear relationship equation: A=0.00133 × C+0.01867, obtain corresponding calculating concentration.Gained calculating concentration and actual concentrations are contrasted, the accurate and reliability of verification method, the results are shown in Table 1.
As can be known from Table 1, calculating concentration is compared with actual concentrations, and relative error is all less than 3%, proves that the inventive method has degree of precision.
The concentration of Polymer Used For Oil Displacement and the comparing result of its actual concentrations that table 1 utilizes the inventive method to detect to obtain
| A value | Calculating concentration (mg/L) | Actual concentrations (mg/L) | Relative error (%) |
| 0.058 | 29.6 | 30 | 1.3 |
| 0.085 | 49.9 | 50 | 0.2 |
| 0.11 | 68.7 | 70 | 1.9 |
| 0.139 | 90.5 | 90 | 0.6 |
| 0.164 | 109.3 | 110 | 0.6 |
| 0.191 | 129.6 | 130 | 0.3 |
| 0.22 | 151.4 | 150 | 1.0 |
| 0.244 | 169.4 | 170 | 0.4 |
| 0.268 | 187.5 | 190 | 1.3 |
| 0.299 | 210.8 | 210 | 0.4 |
| 0.327 | 231.8 | 230 | 0.8 |
| 0.352 | 250.6 | 250 | 0.3 |
| 0.38 | 271.7 | 270 | 0.6 |
| 0.405 | 290.5 | 290 | 0.2 |
The detection of embodiment 2, Polyacrylamides For Enhanced Oil Recoveries concentration
The degree of hydrolysis adopted certain Oil Field is 40%, and molecular weight is that the concentration of 1,800 ten thousand polyacrylamide solutions measures, and step is as follows:
1) 50 DEG C, above-mentioned polyacrylamide dry powder is mixed with on-the-spot injection allocation water under 400rpm condition, hold over night after dissolving completely, obtains 5000mg/L polyacrylamide mother liquor.Through polyacrylamide mother liquor with on-the-spot injection allocation water be diluted to concentration be respectively 0,20,40,60,80,100,120,140,160,180,200,220,240,260,280, the polyacrylamide standard aqueous solution of 300mg/L.
2) 1mL polyacrylamide standard aqueous solution is pipetted in color comparison tube, be diluted with water to 10mL, add 0.5g potassium persulfate powder, 1mL NaOH solution (0.5g/L), shakes up, color comparison tube is placed in WTWCR2200 type heating and decompose device, continue to be heated to 120 DEG C and start timing, after maintaining the temperature at 120 DEG C of 30min, remove enclosing cover, take out color comparison tube and be cooled to 25 DEG C, acutely rock 10min.Mix after adding the HCl solution (0.2g/L) of 1mL in color comparison tube, after leaving standstill natural subsidence 30min, get supernatant.Use quartz colorimetric utensil, on ultraviolet spectrophotometer, make reference with on-the-spot injection allocation water, measure absorbance respectively at wavelength 220nm and 275nm place.The absorbance of zero-dose is designated as A
0, other concentration absorbance be designated as A
x, correct absorbance A according to following formulae discovery:
A
0＝(A
0)
220－2(A
0)
275
A
X＝(A
X)
220－2(A
X)
275
A＝A
X－A
0
With polymkeric substance (polyacrylamide) concentration (C, mg/L) for horizontal ordinate, corresponding A value is ordinate, draws A-C typical curve (Fig. 2).Matching A-C linear relationship equation, determines K and B value: A=0.00125 × C+0.0161.
3) compound concentration be 30,50,70,90,110,130,150,170,190,210,230,250,270, the polyacrylamide solution of 290mg/L, repeat 2) step, the A value of gained is substituted into A-C linear relationship equation: A=0.00125 × C+0.0161, obtain corresponding calculating concentration.Gained calculating concentration and actual concentrations are contrasted, the accurate and reliability of verification method, the results are shown in Table 2.
As can be known from Table 2, calculating concentration is compared with actual concentrations, and relative error is all less than 3%, proves that the inventive method has degree of precision.
The concentration of Polymer Used For Oil Displacement and the comparing result of its actual concentrations that table 2 utilizes the inventive method to detect to obtain
| A value | Calculating concentration (mg/L) | Actual concentrations (mg/L) | Relative error (%) |
| 0.054 | 30.3 | 30 | 1.1 |
| 0.077 | 48.7 | 50 | 2.6 |
| 0.104 | 70.3 | 70 | 0.5 |
| 0.126 | 87.9 | 90 | 2.3 |
| 0.154 | 110.3 | 110 | 0.3 |
| 0.179 | 130.3 | 130 | 0.2 |
| 0.200 | 147.1 | 150 | 1.9 |
| 0.230 | 171.1 | 170 | 0.7 |
| 0.250 | 187.1 | 190 | 1.5 |
| 0.272 | 204.7 | 210 | 2.5 |
| 0.304 | 230.3 | 230 | 0.1 |
| 0.330 | 251.1 | 250 | 0.4 |
| 0.354 | 270.3 | 270 | 0.1 |
| 0.380 | 291.1 | 290 | 0.4 |
The detection of embodiment 3, Polyacrylamides For Enhanced Oil Recoveries concentration
The degree of hydrolysis adopted certain Oil Field is 46%, and molecular weight is that the concentration of the polyacrylamide solution of 2,000 ten thousand detects, and step is as follows:
1) 50 DEG C, above-mentioned polyacrylamide dry powder is mixed with on-the-spot injection allocation water under 400rpm condition, hold over night after dissolving completely, obtains 5000mg/L polyacrylamide mother liquor.Through polyacrylamide mother liquor with on-the-spot injection allocation water be diluted to concentration be respectively 0,20,40,60,80,100,120,140,160,180,200,220,240,260,280, the polyacrylamide standard aqueous solution of 300mg/L.
2) 1mL polyacrylamide standard aqueous solution is pipetted in color comparison tube, be diluted with water to 10mL, add 0.5g potassium persulfate powder, 1mL NaOH solution (0.5g/L), shakes up, color comparison tube is placed in WTWCR2200 type heating and decompose device, continue to be heated to 120 DEG C and start timing, after maintaining the temperature at 120 DEG C of 30min, remove enclosing cover, take out color comparison tube and be cooled to 25 DEG C, acutely rock 10min.Mix after adding the HCl solution (0.2g/L) of 1mL in color comparison tube, after leaving standstill natural subsidence 30min, get supernatant.Use quartz colorimetric utensil, on ultraviolet spectrophotometer, make reference with on-the-spot injection allocation water, measure absorbance respectively at wavelength 220nm and 275nm place.The absorbance of zero-dose is designated as A
0, other concentration absorbance be designated as A
x, correct absorbance A according to following formulae discovery:
A
0＝(A
0)
220－2(A
0)
275
A
X＝(A
X)
220－2(A
X)
275
A＝A
X－A
0
With polymkeric substance (polyacrylamide) concentration (C, mg/L) for horizontal ordinate, corresponding A value is ordinate, draws A-C typical curve (Fig. 3).The linear relationship equation of matching A-C, determines K and B value: A=0.00116 × C+0.02357.
3) compound concentration be 30,50,70,90,110,130,150,170,190,210,230,250,270, the polyacrylamide solution of 290mg/L, repeat 2) step, the A value of gained is substituted into A-C linear relationship equation: A=0.00116 × C+0.02357, obtain corresponding calculating concentration.Gained calculating concentration and actual concentrations are contrasted, the accurate and reliability of verification method, the results are shown in Table 3.
As can be known from Table 3, calculating concentration is compared with actual concentrations, and relative error is all less than 3%, proves that the inventive method has degree of precision.
The concentration of Polymer Used For Oil Displacement and the comparing result of its actual concentrations that table 3 utilizes the inventive method to detect to obtain
| A value | Calculating concentration (mg/L) | Actual concentrations (mg/L) | Relative error (%) |
| 0.059 | 30.2 | 30 | 0.7 |
| 0.081 | 49.7 | 50 | 0.6 |
| 0.106 | 71.3 | 70 | 1.9 |
| 0.127 | 88.9 | 90 | 1.2 |
| 0.153 | 111.5 | 110 | 1.4 |
| 0.175 | 130.3 | 130 | 0.2 |
| 0.199 | 151.1 | 150 | 0.7 |
| 0.223 | 172.1 | 170 | 1.2 |
| 0.242 | 188.1 | 190 | 1.0 |
| 0.266 | 208.7 | 210 | 0.6 |
| 0.291 | 230.3 | 230 | 0.1 |
| 0.315 | 251.1 | 250 | 0.4 |
| 0.337 | 270.6 | 270 | 0.2 |
| 0.362 | 291.5 | 290 | 0.5 |
Claims (8)
1. a detection method for Polymer Used For Oil Displacement concentration, comprises the steps:
(1) on-the-spot injection allocation water is adopted, the Polymer Standards aqueous solution of preparation at least 5 variable concentrations;
(2) in described Polymer Standards aqueous solution, add digestion agent and auxiliary agent respectively, heating is carried out clearing up reaction, adds acid solution after cooling; Utilize ultraviolet spectrophotometer, measure the absorbance of the Polymer Standards solution after clearing up at wavelength 220nm and 275nm place respectively, be designated as (A respectively
x)
220(A
x)
275, the X in formula is the label of described Polymer Standards solution, and X is natural number; Measure the absorbance of reference at wavelength 220nm and 275nm place respectively, be designated as (A respectively
0)
220(A
0)
275;
Described reference is described on-the-spot injection allocation water;
(1) and (2) calculates the correction absorbance of described Polymer Standards aqueous solution and described reference respectively according to the following equation, is designated as A respectively
xand A
0,
A
X＝(A
X)
220－2(A
X)
275(1)
A
0＝(A
0)
220－2(A
0)
275(2)
(3) calculate the difference of the correction absorbance of described Polymer Standards aqueous solution and the correction absorbance of described reference according to the following equation, are designated as A,
A＝A
X－A
0(3)
With the concentration of described Polymer Standards aqueous solution for horizontal ordinate, the difference A of the correction absorbance of described Polymer Standards aqueous solution and the correction absorbance of described reference solution is ordinate, drawing standard curve linear equation;
(3) get Polymer Used For Oil Displacement sample to be measured, repeat above-mentioned steps (2), obtain the difference of the correction absorbance of Polymer Used For Oil Displacement sample to be measured and the correction absorbance of described reference; Namely the concentration of Polymer Used For Oil Displacement sample to be measured is obtained according to described linear equation.
2. detection method according to claim 1, is characterized in that: described polymkeric substance is polyacrylamide.
3. detection method according to claim 2, is characterized in that: the molecular weight of described polyacrylamide is 800 ~ 2,800 ten thousand, and degree of hydrolysis is 10% ~ 50%.
4. the detection method according to any one of claim 1-3, is characterized in that: the concentration of described Polymer Standards aqueous solution is 0 ~ 300mg/L.
5. the detection method according to any one of claim 1-4, is characterized in that: described digestion agent is potassium persulfate, and described auxiliary agent is sodium hydroxide solution;
The addition of described digestion agent and described auxiliary agent is as follows; After described in 1mL, Polymer Standards aqueous solution is diluted with water to 10mL, the addition of described digestion agent is 0.5g, and the addition of described auxiliary agent is 1mL, and the concentration of described auxiliary agent is 0.5g/L.
6. the detection method according to any one of claim 1-5, is characterized in that: described in clear up reaction temperature be 120 ~ 124 DEG C, described in clear up reaction time be 30 ~ 50min;
Described cooling is down to 20 ~ 30 DEG C, and described cooling fully mixes afterwards.
7. the detection method according to any one of claim 1-6, is characterized in that: described acid solution is hydrochloric acid solution;
The addition of described acid solution is as follows: after described in 1mL, Polymer Standards aqueous solution is diluted with water to 10mL, and the addition of described acid solution is 1mL, and the concentration of described acid is 0.2g/L.
8. the detection method according to any one of claim 1-7, is characterized in that: described Polymer Standards aqueous solution is diluted by polymer mother liquor and obtained; Described polymer mother liquor obtains through hold over night after being mixed with described on-the-spot injection allocation water by Polymer Standards product;
The concentration of described polymer mother liquor is 5000 ~ 10000mg/L.
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| CN106290213A (en) * | 2016-08-24 | 2017-01-04 | 中国海洋石油总公司 | The detection method of polymer concentration in a kind of Produced Liquid handling process being suitable to offshore oilfield |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105424884A (en) * | 2015-11-18 | 2016-03-23 | 中国海洋石油总公司 | Method for detecting component concentration of polymer-surfactant binary composite flooding system |
| CN106124283A (en) * | 2016-08-24 | 2016-11-16 | 中国海洋石油总公司 | A kind of remove polymer concentration in Produced Liquid determine nitrogen detection interference factor method |
| CN106290213A (en) * | 2016-08-24 | 2017-01-04 | 中国海洋石油总公司 | The detection method of polymer concentration in a kind of Produced Liquid handling process being suitable to offshore oilfield |
| CN107941648A (en) * | 2016-10-13 | 2018-04-20 | 中国石油化工股份有限公司 | A kind of method of polymer concentration in detection sample |
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| CN107941985A (en) * | 2018-01-12 | 2018-04-20 | 中国海洋石油集团有限公司 | A kind of partially hydrolyzed polyacrylamide (PHPA) suitable for offshore oilfield is birdsed of the same feather flock together the detection method of compound concentration |
| CN111398258A (en) * | 2020-04-29 | 2020-07-10 | 大庆油田有限责任公司 | Quantitative test method and device for polymer in polymer flooding reservoir rock |
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Application publication date: 20150325 |