CN108362794A - The method of chromatography determination polymer adsorbance in adsorbing medium - Google Patents
The method of chromatography determination polymer adsorbance in adsorbing medium Download PDFInfo
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- CN108362794A CN108362794A CN201810118465.5A CN201810118465A CN108362794A CN 108362794 A CN108362794 A CN 108362794A CN 201810118465 A CN201810118465 A CN 201810118465A CN 108362794 A CN108362794 A CN 108362794A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
It is to use pure water or saline different types of polymers standard solution the invention discloses a kind of method of chromatography determination oilfield polymer adsorbance on adsorbing medium；Analysis detection is carried out to polymer solution using liquid chromatography, draws paced work curve；Take adsorbing medium in polymer solution, upper solution is taken to carry out chromatographic determination after shaking adsorption equilibrium, then above-mentioned corresponding paced work curve is brought into according to chromatographic peak area, the concentration for obtaining absorption post-consumer polymer solution, finally according to the adsorbance of the Mass Calculation polymer of the concentration difference of polymer solution, the dosage of polymer solution and adsorbing medium before and after absorption.The present invention is realized using liquid chromatography and carries out analysis detection to low concentration polymer solution, detection performance is stable, it is sensitive it is quick, analyze speed is fast, test result is reproducible, quantitative error is small, retest relative standard deviation is less than 5 %, can meet the needs that oilfield chemistry drives the tracking and monitoring of polymer concentration variation used completely.
Description
Technical field
The test method of adsorbance that the present invention relates to a kind of polymer in adsorbing medium more particularly to chromatography determination are poly-
The method for closing adsorbance of the object in adsorbing medium belongs to oilfield chemistry and drives polymer analysis monitoring technology field.
Background technology
During tertiary oil recovery, polymer flooding can significantly improve oil recovery efficiency, become oil field development and improve recovery ratio
Technical way, and be widely popularized and applied in each elephant.China has become uses polymer flooding skill in the world
Art is largest, increases the best country of effect, and technique of polymer flooding becomes the important technology of China's oil Sustainable high yield stable yields
Measure.Polymer can occur to adsorb or be detained loss in the migration process of stratum, cause polymer concentration and viscosity to reduce, cause
The system formulation composition of different polymer changes, and Oil Displacing Capacity generates difference.Suction of the Study Polymer Melts in adsorbing medium
Attached performance difference can provide corresponding data theory basis for polymer flooding preliminary screening polymer, there is the guidance of reality to make
With.
Currently, researcher carries out analysis detection using starch-cadmium iodine colorimetric method to polymer solution concentration, operation
It is relatively cumbersome；In addition, for high concentration（>1000 mg/L）Polymer solution, per sub-sampling when be difficult to ensure or can not obtain
Uniform sample system necessarily leads to the unexpected property of result.And for low concentration（200 mg/L or less）Polymer is molten
Liquid carries out analysis detection, error then bigger.
Invention content
The purpose of the present invention is be directed to be unable to Accurate Determining oilfield polymer in the prior art and adsorb on adsorbing medium
The problem of amount, provides a kind of method of chromatography determination oilfield polymer adsorbance in adsorbing medium.
（1）Preparing standard solution
By polymer pure water or saline at solution, magnetic agitation is used as mother liquor after so that polymer is completely dissolved, then uses salt
Mother liquor is diluted to the polymer solution of serial various concentration by water.
Above-mentioned polymer is 10,000,000 polyacrylamides, 15,000,000 polyacrylamides, 25,000,000 polyacrylamides, hydrophobic forms
Close polymer, sulfonic acid type acrylamide.
The salinity of brine is 5000-30000mg/L；Polymer solution concentration ranging from 10-200mg/L.
Fig. 1 is the liquid chromatogram of polymer solution, first chromatographic peak in chromatogram（Retention time is on the left sides 1.8min
It is right）As polymer chromatography peak is kept completely separate with the small molecules such as inorganic salts coexist, and is conducive to the accurate quantitative analysis point of polymer
Analysis.
（2）Draw paced work curve
Chromatography is carried out by sample to be tested of various concentration standard solution, is painted according to sample concentration and corresponding chromatographic peak area
Formulation amount working curve；Chromatographiccondition is：Mobile phase is the biphosphate sodium water solution of 0.25mol/L, flow velocity 1mL/
Min, Detection wavelength 200nm, sample size 20uL.
（3）Concentration Testing
Adsorbing medium is added in a polymer solution, upper solution is taken after shaking absorption 0.5-6h, crosses 0.45um filter membranes, it is then right
Polymer solution after absorption carries out chromatography and brings above-mentioned corresponding paced work curve into then according to chromatographic peak area, obtain
The concentration of post-consumer polymer solution must be adsorbed.
Adsorbing medium is porous adsorbing medium（Such as silica gel）Or solid adsorbing medium（Such as oil-sand）；Adsorbing medium and polymer
The mass volume ratio of solution is 1:10-1:30 mL/g.
Chromatographiccondition is：Mobile phase is the biphosphate sodium water solution of 0.25mol/L, flow velocity 1mL/min, detection
Wavelength is 200nm, sample size 20uL.
（4）Adsorbance calculates
According to the concentration difference of polymer solution, the quality of the dosage of polymer solution and adsorbing medium before and after absorption, count as the following formula
Calculate adsorbance of the polymer on adsorbing medium：
Г-Polymer adsorption amount, unit：mg/g
C 0 - absorption prepolymer concentration, unit：mg/L
Ce- absorption post-consumer polymer concentration, unit：mg/L
V- polymer solution volume, unit：mL
M- adsorbing medium quality, unit：g.
The present invention has the advantages that compared with the prior art：Using liquid chromatography, realize to relatively low dense
Degree（About 200 mg/L）Polymer solution carries out analysis detection, detection performance is stable, it is sensitive it is quick, analyze speed is fast（Complete one
Secondary analysis detects about 3 min）, test result is reproducible, quantitative error is small, and retest relative standard deviation is less than 5 %, complete
The needs that oilfield chemistry drives the tracking and monitoring of polymer concentration variation used can be met entirely, inhaled according to different types of polymers
Adsorbance comparison on attached medium helps to provide corresponding data theory basis for polymer flooding preliminary screening polymer, is
Delay Loss Research of the later stage polymer in oil reservoir gap provides reference frame and correction data.
Description of the drawings
Fig. 1 is the liquid chromatogram of polymer solution in the present invention.
Fig. 2 is 1 paced work curve of the embodiment of the present invention.
Fig. 3 is 2 paced work curve of the embodiment of the present invention.
Fig. 4 is 3 paced work curve of the embodiment of the present invention.
Fig. 5 is 4 paced work curve of the embodiment of the present invention.
Fig. 6 is 5 paced work curve of the embodiment of the present invention.
Specific implementation mode
Used instrument and reagent are as follows in the examples below：
High performance liquid chromatograph, Agilent 1100, the U.S.；Polymer dedicated analysis column（5 μm, 150mm × 4.6mm）, the Chinese Academy of Sciences
Lanzhou Chemical Physics research institute.
Silica gel, Qingdao Marine Chemical Co., Ltd.；Oil-sand, Sinopec Shengli Oil Field branch company；10000000 polyacrylamides
Amine, 15,000,000 polyacrylamides, 25,000,000 polyacrylamides, hydrophobic associated polymer, sulfonic acid type acrylamide, Sinopec
Shengli Oil Field branch company；Sodium dihydrogen phosphate, sodium chloride analyze pure, silver beneficial friend's chemical reagent Co., Ltd；Distilled water by
Milli-Q systems obtain.
Embodiment 1
（1）Preparing standard solution：It is 10,000,000 polyacrylamide polymers solid particle to take 0.04g molecular weight, under stiring
It is slowly added in the brine of salinity 20000mg/L, continues magnetic agitation for 24 hours, keep polymer dissolving complete, it is molten as polymer
Liquid mother liquor.Mother liquor is diluted with the brine of salinity 20000mg/L, compound concentration is respectively the mark of 10,25,50,100,200mg/L
Quasi- solution.
（2）Draw paced work curve：Chromatographiccondition：Mobile phase is the biphosphate sodium water solution of 0.25mol/L,
Flow velocity is 1mL/min, Detection wavelength 200nm, sample size 20uL.Color is carried out by sample to be tested of various concentration standard solution
Spectrum analysis carries out the drafting of paced work curve according to sample concentration and corresponding chromatographic peak area（With Polymer Standards solution
A concentration of abscissa, chromatographic peak area is ordinate）.Each concentration point detects 3 times, is averaged.Polymer 1 quantitatively returns
Curve is shown in Table 1.
（3）Concentration Testing：Take 1g adsorbing mediums（Respectively 200 ~ 300 mesh silica gel, 100 ~ 200 mesh silica gel, 70 ~ 100 mesh oil
Sand）In 50mL conical flasks, be separately added into 10,20,30mL polymer solution mother liquors, vibrate 3h, upper solution taken to cross 0.45um
The laggard chromatography of filter membrane：Mobile phase is the biphosphate sodium water solution of 0.25mol/L, and flow velocity 1mL/min, Detection wavelength is
200nm, sample size 20uL.According to chromatographic peak area, paced work curve is brought into, obtain the dense of absorption post-consumer polymer solution
Degree.
（4）Adsorbance calculates
According to above-mentioned adsorbance calculation formula, adsorbance of the polymer on different adsorbing mediums is calculated.It the results are shown in Table 2-4.
Embodiment 2
Except step（1）It is added in preparing standard solution outside the polyacrylamide that molecular weight is 15,000,000, remaining step is all the same as implementation
Example 1.The quantitative regression result of the polymer samples is shown in Table 1；Adsorbance test result of the polymer in different medium is shown in Table
2-4。
Embodiment 3
Except step（1）It is added in preparing standard solution outside the polyacrylamide that molecular weight is 25,000,000, remaining step is all the same as implementation
Example 1.The quantitative regression result of the polymer samples is shown in Table 1；Adsorbance test result of the polymer in different medium is shown in Table
2-4。
Embodiment 4
Except step（1）It is added outside hydrophobic associated polymer in preparing standard solution, remaining step is all the same as embodiment 1.The polymer
The quantitative regression result of sample is shown in Table 1；Adsorbance test result of the polymer in different medium is shown in Table 2-4.
Embodiment 5
Except step（1）It is added outside sulfonic acid type acrylamide in preparing standard solution, remaining step is all the same as embodiment 1.The polymerization
The quantitative regression result of object sample is shown in Table 1；Adsorbance test result of the polymer in different medium is shown in Table 2-4.
The quantitative regression result of 5 polymer samples to be measured is listed in table 1；Adsorbance of the polymer in different medium
Test result is listed in table 2-4 respectively.
1 polymer 1-5 of table quantifies regression curve
2 Polymer adsorption of table measures test result（200 ~ 300 mesh silica gel）
3 Polymer adsorption of table measures test result（100 ~ 200 mesh silica gel）
4 Polymer adsorption of table measures test result（70 ~ 100 mesh oil-sands）
By table 1 as it can be seen that the quantitative regression equation related coefficient of 5 kinds of polymer samples to be measured is good, measured value and the real phase with value
5% is less than to standard deviation, illustrates that the assay method is accurate and reliable.The above experiment is repeated using the method, the results showed that, it should
Method all has high accuracy to various concentration point, and reproducibility is preferable, and Determination Limit can be down to 2mg/L.
By table 2-4 as it can be seen that adsorbance of the polymer on Bio-sil and oil-sand medium is relatively low, or even without absorption；Phase
Comparatively, the molecular weight of polymer is bigger, adsorbance is higher, and hydrophobic grouping is more, and adsorbance is lower.The molecular weight of polymer
It is higher, cause polymer molecule to be difficult into the hole on adsorbing medium surface, therefore whether adsorbing medium has porosity,
To its absorption property without substantial influence.The influence of adsorbing medium particle size, temperature height to Polymer adsorption amount is weaker, related
Investigation factors above can be ignored in research process.In addition, polymer does not have on silica gel absorption medium and oil-sand adsorbing medium
Notable difference is shown, two media is more similar to the absorption property of polymer, shows that the porosity of adsorbing medium is not
Influence the principal element of Polymer adsorption performance.
Claims (7)
1. the method for chromatography determination polymer adsorbance in adsorbing medium, comprises the following steps that：
（1）Preparing standard solution：By polymer pure water or saline at solution, after magnetic agitation makes polymer be completely dissolved
As mother liquor, then mother liquor is diluted to brine the polymer solution of serial various concentration；
（2）Draw paced work curve：Chromatography is carried out by sample to be tested of various concentration standard solution, according to sample concentration
Paced work curve is drawn with corresponding chromatographic peak area；
（3）Concentration Testing：Adsorbing medium is added in a polymer solution, upper solution, mistake are taken after shaking absorption 0.5-6h
Then 0.45um filter membranes carry out chromatography to the polymer solution after absorption, then according to chromatographic peak area, it is above-mentioned right to bring into
Paced work curve is answered, the concentration of absorption post-consumer polymer solution is obtained；
（4）Adsorbance calculates：According to the concentration difference of polymer solution before and after absorption, the dosage of polymer solution and adsorbing medium
Adsorbance of the polymer on adsorbing medium is calculated as follows in quality：
Г-Polymer adsorption amount, unit：mg/g
C 0 - absorption prepolymer concentration, unit：mg/L
Ce- absorption post-consumer polymer concentration, unit：mg/L
V- polymer solution volume, unit：mL
M- adsorbing medium quality, unit：g.
2. the method for chromatography determination polymer adsorbance in adsorbing medium as described in claim 1, it is characterised in that：Step
（1）In, polymer is 10,000,000 polyacrylamides, 15,000,000 polyacrylamides, 25,000,000 polyacrylamides, hydrophobic association polymerization
Object, sulfonic acid type acrylamide.
3. the method for chromatography determination polymer adsorbance in adsorbing medium as described in claim 1, it is characterised in that：Step
（1）In, the salinity of brine is 5000-30000mg/L.
4. the method for chromatography determination polymer adsorbance in adsorbing medium as described in claim 1, it is characterised in that：Step
（1）In, polymer solution concentration ranging from 10-200mg/L.
5. the method for chromatography determination polymer adsorbance in adsorbing medium as described in claim 1, it is characterised in that：Step
（2）、（3）In, chromatographiccondition is：Mobile phase is the biphosphate sodium water solution of 0.25mol/L, flow velocity 1mL/min, inspection
Survey wavelength is 200nm, sample size 20uL.
6. the method for chromatography determination polymer adsorbance in adsorbing medium as described in claim 1, it is characterised in that：Step
（3）In, adsorbing medium is porous adsorbing medium or solid adsorbing medium.
7. the method for chromatography determination polymer adsorbance in adsorbing medium as claimed in claim 6, it is characterised in that：Absorption
The mass volume ratio of medium and polymer solution is 1:10-1:30 mL/ g.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109444282A (en) * | 2018-12-06 | 2019-03-08 | 中国科学院兰州化学物理研究所 | The method of active matter content in liquid chromatogram measuring Daqing oil field petroleum sulfonate sample |
| CN111307646A (en) * | 2020-02-27 | 2020-06-19 | 西南石油大学 | Method for measuring adsorption capacity of polymer treating agent in brine drilling fluid on clay surface |
| CN112114078A (en) * | 2020-08-21 | 2020-12-22 | 中国科学院兰州化学物理研究所 | Analysis method for simultaneously detecting content of polyacrylamide polymer and hydrophobically associating polymer |
| CN113029992A (en) * | 2021-03-03 | 2021-06-25 | 重庆科技学院 | Experimental device and method for dynamic adsorption of viscoelastic fluid on surface of medium |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109444282A (en) * | 2018-12-06 | 2019-03-08 | 中国科学院兰州化学物理研究所 | The method of active matter content in liquid chromatogram measuring Daqing oil field petroleum sulfonate sample |
| CN111307646A (en) * | 2020-02-27 | 2020-06-19 | 西南石油大学 | Method for measuring adsorption capacity of polymer treating agent in brine drilling fluid on clay surface |
| CN111307646B (en) * | 2020-02-27 | 2022-02-01 | 西南石油大学 | Method for measuring adsorption capacity of polymer treating agent in brine drilling fluid on clay surface |
| CN112114078A (en) * | 2020-08-21 | 2020-12-22 | 中国科学院兰州化学物理研究所 | Analysis method for simultaneously detecting content of polyacrylamide polymer and hydrophobically associating polymer |
| CN113029992A (en) * | 2021-03-03 | 2021-06-25 | 重庆科技学院 | Experimental device and method for dynamic adsorption of viscoelastic fluid on surface of medium |
| CN113029992B (en) * | 2021-03-03 | 2022-01-18 | 重庆科技学院 | Experimental device and method for dynamic adsorption of viscoelastic fluid on surface of medium |
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