CN105424533A - Hydrolysis degree determination method for polyacrylamide with high hydrolysis degree - Google Patents
Hydrolysis degree determination method for polyacrylamide with high hydrolysis degree Download PDFInfo
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Abstract
The invention relates to a hydrolysis degree determination method for polyacrylamide with a high hydrolysis degree. According to the method, a slightly excessive amount of sodium hydroxide solution and a polymer solution are subjected to a replacement reaction first to make all ammonium carboxylate radicals in a polymer replaced by sodium carboxylate radicals, the solution obtained after the reaction is subjected to extraction with absolute ethyl alcohol, extracted components are fired through a firing method until the polymer is completely ashed, the mass of ash is weighed, the ash is mostly composed of sodium carbonate, the mole number of the ammonium carboxylate radicals subjected to the replacement reaction in the polymer can be obtained according to the mass of the sodium carbonate, and then the hydrolysis degree can be obtained. Compared with a common methyl orange and indigo carmine titration method, the adopted ash determination method is good in reproducibility and avoids the influence of human factors resulting from judgment of a titration end point in the titration method. The method is used for hydrolysis degree determination of the polyacrylamide with a high hydrolysis degree. By the adoption of the determination method, the adopted reagent is free of toxicity, pollution to the environment is avoided, operation is easy and convenient, reproducibility is good, and measuring accuracy is high.
Description
Technical field
The invention belongs to quantitative test field, be specifically related to a kind of degree of hydrolysis assay method of high degree of hydrolysis polyacrylamide.
Background technology
Partially hydrolyzed polyacrylamide (HPAM) is the synthesizing water-solubility high polymer chemistry product that turnout is maximum in the world at present, is widely used in many production divisions such as improving oil recovery, drilling well, ore dressing, papermaking, medicine, water treatment.
HPAM is obtained through basic hydrolysis by polyacrylamide (PAM), and in hydrolysate, acrylates chain link accounts for the percentage of allylamine chain number in PAM, is the degree of hydrolysis of PAM.Generally add different alkali numbers, the HPAM of different degree of hydrolysis can be obtained.
Degree of hydrolysis is a basic parameter of HPAM structural characterization, also be the important Testing index evaluating dry powder class polyacrylamide product quality simultaneously, its size directly affects the aggregated structure of polymer solution, the important parameters such as rheological property and chemical machinery stability, particularly important in the application of high temperature and high salt oil deposit.HPAM is as chemical thickening agent, and a small amount of HPAM is dissolved in injection water just can significantly improve solution viscosity, is conducive to reducing oil and water mobility ratio, improves sweep efficiency, thus improve oil recovery factor.The HPAM average molecular mass that oil field is commonly used is millions of to up to ten million, and degree of hydrolysis is 20%-30%.The polymeric water-soluble that degree of hydrolysis is too little is poor, and the too large polymkeric substance of degree of hydrolysis is strong to salt, hardness, shearing force susceptibility.Therefore, measure the degree of hydrolysis of HPAM quickly and accurately, for its product quality of control, assess its solubility property and oil displacement efficiency all has important practical significance.
The degree of hydrolysis assay method that present stage is commonly used is methyl orange and sodium indigotindisulfonate titrimetry.It is mainly applicable to the mensuration of conventional Lower degrees of hydrolysis polyacrylamide amine product, and the method to there is sampling amount few, hydrochloric acid standard solution consumption is few, do not deduct blank impact and when measuring high degree of hydrolysis sample, during titration end-point, color change is not obvious, terminal is stalled for time longer, harsher to the requirement of water quality and sample.When Lower degrees of hydrolysis sample tests, testing result is higher, and when sample is high degree of hydrolysis, testing result is on the low side and deviation is larger.
Summary of the invention
The object of the present invention is to provide that a kind of accuracy is high, error is little, the method for the mensuration polyacrylamide hydrolysis degree of favorable reproducibility.
The technical solution adopted for the present invention to solve the technical problems is: a kind of method measuring polyacrylamide hydrolysis degree, comprises the following steps:
1) first measure the solid content of polyacrylamide amine product, be designated as S;
2) in 500ml beaker, add 100g pure water, start magnetic stirring apparatus, make liquid in beaker form 2ml whirlpool, accurately take 1.00g Laemmli sample with difference assay, be accurate to 0.0001g, be designated as m
1, sample is slowly joined in beaker, starts to add excess sodium hydroxide solution in a subtle way after stirring 30min, until sample dissolves completely, after being stirred evenly by sample, carry out extraction with organic solvent stand-by;
3) accurately take crucible quality, be accurate to 0.0001g, be designated as m
2, the crucible filling extract is placed on universal electronic stove slowly red-hot, notes avoiding burning, after extract carbonization, crucible is put into chamber type electric resistance furnace, at 600 DEG C, place 3h make it complete ashing and to constant weight;
4) take out crucible, be placed in exsiccator, cool after 30 minutes and weigh, be designated as m
3, be accurate to 0.0001g, degree of hydrolysis is calculated as follows:
In formula: HD-degree of hydrolysis, %;
M
1the quality of-Laemmli sample, g;
The solid content of S-Laemmli sample, %;
M
2the quality of-crucible, g;
M
3-crucible adds the quality of ash content, g.
Particularly, described step 1) in the determination step of polyacrylamide solid content as follows: get a clean measuring cup, at 105 DEG C ± 2 DEG C, be dried to constant weight, record its quality, be accurate to 0.001g; In the measuring cup of constant weight, add 0.99 ~ 1.01g sample, be accurate to 0.0001g; The measuring cup weighing up sample being placed in temperature is in the baking oven of 120 DEG C, heat drying 2 hours; Take out measuring cup, be placed in exsiccator, cool after 30 minutes and weigh, be accurate to 0.0001g; Solid content percentage is calculated as follows:
In formula: the solid content of S-sample, 100%
Sample mass after m-drying, g
M
0-dry front sample mass, g
Particularly, described step 2) in micro-excess sodium hydroxide solution add several times.
Particularly, described step 2) in organic solvent be the organic solvent of insoluble polyacrylamide, be preferably absolute ethyl alcohol.
Micro-excessive sodium hydroxide solution and polymer solution is first used to carry out displacement reaction in the present invention, the ammonium carboxylic acid salt groups in polymkeric substance is made all to be replaced into sodium carboxylate groups, reacted solution absolute ethyl alcohol extracts, by the method for calcination, the component after extraction is carried out calcination again, until after the complete ashing of polymkeric substance, take the quality of ash content, the component of ash content is sodium carbonate substantially entirely, the molal quantity of the ammonium carboxylic acid salt groups that displacement reaction occurs can be tried to achieve in polymkeric substance according to the quality of sodium carbonate, and then obtain degree of hydrolysis.With conventional methyl orange compared with sodium indigotindisulfonate titrimetry, the Ash determination method favorable reproducibility that the present invention adopts, avoids in titrimetry and judges titration end-point and the impact of the human factor of generation.Degree of hydrolysis for high degree of hydrolysis polyacrylamide measures and provides that a kind of agents useful for same is nontoxic, environmentally safe, easy and simple to handle, favorable reproducibility, measuring accuracy and the high assay method of accuracy.
Embodiment
Be below specific embodiments of the invention, technical scheme of the present invention is described further, but protection scope of the present invention is not limited to these embodiments.Every do not deviate from the present invention's design change or equivalent substituting include within protection scope of the present invention.
The sample adopted in following examples is the polyacrylamide of degree of hydrolysis 80.00%, and sample is 61.58% through the degree of hydrolysis that titrimetry records.
Embodiment 1
Get the 500ml beaker of a dried and clean, take 100.00g pure water and add beaker, stir under the rotating speed of 400r/min under beaker being placed in paddle stirrer.Accurately take the sample of the polyacrylamide of 1.00g, be designated as m
1, sample is slowly joined in beaker.Start the sodium hydroxide solution that every 10min adds 1ml5% after stirring 30min, amount to and add 9ml.After stirring 2h, stop stirring, beaker is taken out from paddle stirrer.After being stirred evenly by sample, in the beaker of average mark to 5 500ml, the absolute ethyl alcohol adding 3 times amount respectively extracts.After 4h extraction completely, extract is taken out and shred.Accurately take crucible quality, be designated as m
2, the crucible filling extract is placed on universal electronic stove slowly red-hot, notes avoiding burning, after extract carbonization, crucible is put into chamber type electric resistance furnace, at 600 DEG C, place 3h make it complete ashing and to constant weight.Take out crucible, be placed in exsiccator, cool weighing after 30 minutes and be accurate to 0.0001g, be designated as m
3.Gained S=89.64%, m
1=1.0002g, m
2=16.6258g, m
3=17.0568g, HD=76.96%.
Embodiment 2
Get the 500ml beaker of a dried and clean, take 100.00g pure water and add beaker, stir under the rotating speed of 400r/min under beaker being placed in paddle stirrer.Accurately take the sample of the polyacrylamide of 1.00g, be designated as m
1, sample is slowly joined in beaker.Start the sodium hydroxide solution that every 10min adds 1ml10% after stirring 30min, amount to and add 5ml.After stirring 2h, stop stirring, beaker is taken out from paddle stirrer.After being stirred evenly by sample, in the beaker of average mark to 5 500ml, the absolute ethyl alcohol adding 3 times amount respectively extracts.After 4h extraction completely, extract is taken out and shred.Accurately take crucible quality, be designated as m
2, the crucible filling extract is placed on universal electronic stove slowly red-hot, notes avoiding burning, after extract carbonization, crucible is put into chamber type electric resistance furnace, at 600 DEG C, place 3h make it complete ashing and to constant weight.Take out crucible, be placed in exsiccator, cool weighing after 30 minutes and be accurate to 0.0001g, be designated as m
3.Gained S=89.64%, m
1=1.0001g, m
2=15.3041g, m
3=15.7562g, HD=81.51%.
Embodiment 3
Get the 500ml beaker of a dried and clean, take 100.00g pure water and add beaker, stir under the rotating speed of 400r/min under beaker being placed in paddle stirrer.Accurately take the sample of the polyacrylamide of 1.00g, be designated as m
1, sample is slowly joined in beaker.Start the sodium hydroxide solution that every 10min adds 1ml20% after stirring 30min, amount to and add 3ml.After stirring 2h, stop stirring, beaker is taken out from paddle stirrer.After being stirred evenly by sample, in the beaker of average mark to 5 500ml, the absolute ethyl alcohol adding 3 times amount respectively extracts.After 4h extraction completely, extract is taken out and shred.Accurately take crucible quality, be designated as m
2, the crucible filling extract is placed on universal electronic stove slowly red-hot, notes avoiding burning, after extract carbonization, crucible is put into chamber type electric resistance furnace, at 600 DEG C, place 3h make it complete ashing and to constant weight.Take out crucible, be placed in exsiccator, cool weighing after 30 minutes and be accurate to 0.0001g, be designated as m
3.Gained S=89.64%, m
1=1.0001g, m
2=16.1229g, m
3=16.5783, HD=82.26%.
To sum up, measure the degree of hydrolysis of polyacrylamide by method of the present invention, accuracy is high, and error is little, and favorable reproducibility is that the degree of hydrolysis mensuration of high degree of hydrolysis polyacrylamide provides a kind of new thinking and countermeasure.
Claims (5)
1. the degree of hydrolysis assay method of high degree of hydrolysis polyacrylamide, is characterized in that, comprise the following steps:
1) first measure the solid content of polyacrylamide amine product, be designated as S;
2) in 500ml beaker, add 100g pure water, start magnetic stirring apparatus, make liquid in beaker form 2ml whirlpool, accurately take 1.00g Laemmli sample with difference assay, be accurate to 0.0001g, be designated as m
1, sample is slowly joined in beaker, starts to add excess sodium hydroxide solution in a subtle way after stirring 30min, until sample dissolves completely, after being stirred evenly by sample, carry out extraction with organic solvent stand-by;
3) accurately take crucible quality, be accurate to 0.0001g, be designated as m
2, the crucible filling extract is placed on universal electronic stove slowly red-hot, notes avoiding burning, after extract carbonization, crucible is put into chamber type electric resistance furnace, at 600 DEG C, place 3h make it complete ashing and to constant weight;
4) take out crucible, be placed in exsiccator, cool after 30 minutes and weigh, be designated as m
3, be accurate to 0.0001g, degree of hydrolysis is calculated as follows:
In formula: HD-degree of hydrolysis, %;
M
1the quality of-Laemmli sample, g;
The solid content of S-Laemmli sample, %;
M
2the quality of-crucible, g;
M
3-crucible adds the quality of ash content, g.
2. the method for mensuration polyacrylamide hydrolysis degree according to claim 1, is characterized in that, described step 1) in the determination step of polyacrylamide solid content as follows:
Get a clean measuring cup, at 105 DEG C ± 2 DEG C, be dried to constant weight, record its quality, be accurate to 0.001g; In the measuring cup of constant weight, add 0.99 ~ 1.01g sample, be accurate to 0.0001g; The measuring cup weighing up sample being placed in temperature is in the baking oven of 120 DEG C, heat drying 2 hours; Take out measuring cup, be placed in exsiccator, cool after 30 minutes and weigh, be accurate to 0.0001g; Solid content percentage is calculated as follows:
In formula: the solid content of S-sample, 100%
Sample mass after m-drying, g
M
0-dry front sample mass, g.
3. the method for mensuration polyacrylamide hydrolysis degree according to claim 1, is characterized in that, described step 2) in micro-excess sodium hydroxide solution add several times.
4. the method for mensuration polyacrylamide hydrolysis degree according to claim 1, is characterized in that, described step 2) in organic solvent be the organic solvent of insoluble polyacrylamide.
5. the method for mensuration polyacrylamide hydrolysis degree according to claim 4, is characterized in that, described organic solvent is absolute ethyl alcohol.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106979905A (en) * | 2017-03-31 | 2017-07-25 | 中国海洋石油总公司 | It is quick to characterize polyacrylamide polymers for oil displacement product quality stability approach and application |
| CN107941647A (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 |
| CN109557247A (en) * | 2019-01-18 | 2019-04-02 | 王雷 | A kind of degree of hydrolysis measuring instrument and its measurement method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107941647A (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 |
| CN106979905A (en) * | 2017-03-31 | 2017-07-25 | 中国海洋石油总公司 | It is quick to characterize polyacrylamide polymers for oil displacement product quality stability approach and application |
| CN106979905B (en) * | 2017-03-31 | 2019-07-26 | 中国海洋石油总公司 | Quickly characterization polyacrylamide polymers for oil displacement stable product quality method and application |
| CN109557247A (en) * | 2019-01-18 | 2019-04-02 | 王雷 | A kind of degree of hydrolysis measuring instrument and its measurement method |
| CN109557247B (en) * | 2019-01-18 | 2024-04-12 | 北京盛维基业科技有限公司 | Hydrolysis degree measuring instrument and measuring method thereof |
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