CN105954147A - Hydrophobic associated polymer intrinsic viscosity determining method - Google Patents
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- CN105954147A CN105954147A CN201610389979.5A CN201610389979A CN105954147A CN 105954147 A CN105954147 A CN 105954147A CN 201610389979 A CN201610389979 A CN 201610389979A CN 105954147 A CN105954147 A CN 105954147A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
- G01N11/02—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material
- G01N11/04—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material through a restricted passage, e.g. tube, aperture
- G01N11/06—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material through a restricted passage, e.g. tube, aperture by timing the outflow of a known quantity
Abstract
The invention relates to a hydrophobic associated polymer intrinsic viscosity determining method. The hydrophobic associated polymer intrinsic viscosity determining method includes the following steps that step S10, a hydrophobic associated polymer solution is prepared, cyclodextrin and a sodium chloride solution are added to the hydrophobic associated polymer solution to prepare a to-be-tested sample solution; step S20, a sodium chloride solution is added to the to-be-tested sample solution, and the mass concentrations C, specific viscosities eta sp and reduced viscosities eta sp/C of the to-be-tested sample solution and the mixed solution are respectively measured; step S30, a excel graphical method is used for determining the intrinsic viscosity [eta]; step S40, the intrinsic viscosity [eta] is inspected. The hydrophobic associated polymer intrinsic viscosity determining method has the advantages that the characteristics of having hydrophobic cavities of the cyclodextrin are utilized to include hydrophobic groups and shield a hydrophobic associating effect, and the influence on intrinsic viscosity determination of the hydrophobic associated polymer of super-molecular aggregation formed by the associating effect is avoided; the measuring accuracy is high, the cyclodextrin has no surface activity, the measuring accuracy is not affected even if the quantity is excessive.
Description
Technical field
The present invention relates to a kind of hydrophobic associated polymer Intrinsic Viscosity Measurements method.
Background technology
Hydrophobic associated polymer refers to introduce the one of very small amount hydrophobic group on the main chain of traditional water-soluble polymer
Class new water soluble polymers.Owing to the association between its hydrophobic group can form dynamic physical cross-linked network structure, tool
There are the tackifying ability more higher than conventional polymer and shear thinning behavior, coatings industry and petroleum industry have a wide range of applications
Prospect.
In hydrophobic associated polymer strand, the association with interchain is strong and weak, constantly changes with polymer concentration change
Become.Intramolecular association occupies leading at low concentrations, hydrophobic associated polymer dimensional contraction；And Interpolymer Association in higher concentrations
Occupying leading, aggregate size increases with concentration and constantly increases.This gives the performance characterization of hydrophobic associated polymer, such as molecular weight
With the measurement etc. of intrinsic viscosity ([η]), bring the biggest difficulty.Molecular weight be evaluate polymer performance important performance indexes it
One.The main method of experimental determination Molecular Weight for Polyacrylamide has sedimentation, osmometry, light scattering method and viscosity method
Deng.The more commonly used method is to measure the intrinsic viscosity of polymer with viscosity method, intrinsic viscosity representation unit mass polymer
The relative size of molecule shared hydrodynamic volume in the solution, it directly affects the rheological property of polymer.To conventional portion
For dividing hydrolyzed polyacrylamide, its intrinsic viscosity generally uses national standard.In national standard, with the chlorine of 1.00mol/L
Change sodium solution be solvent can the polyelectrolyte effect of effective masked segment hydrolyzed polyacrylamide, the data recorded can be accurate
The intrinsic viscosity of reactive polymeric thing.But for hydrophobic associated polymer, adding of salt promotes between hydrophobic group
Association, multiple association polymers are commonly formed polymolecular aggregation, cause the data recorded can not accurately reflect hydrophobic forming
Close hydrodynamic volume shared by polymer molecule.At present, molecular weight or its characteristic of hydrophobic associated polymer are either measured
Viscosity number, main technical thought is all to eliminate the association between hydrophobic group, makes hydrophobic associated polymer in the solution
Exist with single stranded form.Conventional method has: (1) uses suitable solvent or cosolvent, such as methanol, Methanamide, N, N '-diformazan
Base Methanamide, oxolane etc.；(3) surfactant shielding heat resistance and salt tolerance is added.These methods are respectively arranged with its quality, use
The method of cosolvent can eliminate the association between hydrophobic group, but also can reduce the dissolubility of sodium chloride.Sodium chloride addition is not
Can cause completely polymer molecule segment electrostatic repulsion can not be thus completely shielded, cause experimental error.And add surface and live
The difficulty of the method for property agent is to determine the dosage of surfactant.A small amount of surfactant can not shield hydrophobic group completely
Group, and excess surface active agent self forms micelle, affects experimental result.
Summary of the invention
The technical problem to be solved is to provide a kind of hydrophobic associated polymer Intrinsic Viscosity Measurements method, the party
Method has the following characteristics that the cyclodextrin that D-glucopyranosyl is formed by connecting with α-Isosorbide-5-Nitrae-glucoside bond, has hydrophobic internal cavities
With hydrophilic outer wall, energy inclusion hydrophobic group, the mutual association between suppression hydrophobic group.And cyclodextrin self does not have table
Face activity, will not form micelle in the solution.Therefore, cyclodextrin can eliminate the association of hydrophobic group, even if excess is also
Do not interfere with experimental result.The hydrophobic associated polymer intrinsic viscosity recorded has higher measurement accuracy, can reflect hydrophobic forming
Close polymer strand characteristic.
The present invention solves above-mentioned technical problem and be the technical scheme is that a kind of hydrophobic associated polymer intrinsic viscosity is surveyed
Determine method, comprise the following steps:
Step S10, preparation hydrophobic association polymer solution, add Cyclodextrin, chlorination in hydrophobic association polymer solution
Sodium solution, makes sample to be tested solution；
Step S20, in the sample to be tested solution of hydrophobic associated polymer, add sodium chloride solution, then measure thin respectively
The sample to be tested solution of water association polymer and mass concentration C of mixed solution, specific viscosity ηsp, reduced viscosity ηsp/C；
Step S30, determine intrinsic viscosity by excel diagram method；
Step S40, intrinsic viscosity are tested.
Further, the concretely comprising the following steps of described step S10:
Step S101, the solid content S of configuration hydrophobic associated polymer sample1；
Step S102, in hydrophobic associated polymer style add distilled water be configured to hydrophobic association polymer solution；
Step S103, addition cyclodextrin are configured to cyclodextrin/hydrophobic association polymer solution；
Step S104, cyclodextrin/hydrophobic association polymer solution and sodium chloride solution are positioned in 100mL volumetric flask,
And with distilled water diluting to scale, it is configured to sample to be tested solution；
Step S105, by sample to be tested solution with glass core funnel filter.
Further, described step S102 is particularly as follows: gather with the hydrophobic association that distilled water configuration quality mark is 0.2%
Polymer solution, stirring at low speed is placed 24 hours after within 2 hours, being completely dissolved to hydrophobic associated polymer sample.
Further, described step S103 is particularly as follows: weigh cyclodextrin sample solid content S2, it is added into step S102
In the hydrophobic association polymer solution that middle configuration is good, place 2 hours after being completely dissolved.
Further, the step of described step S104 particularly as follows: accurately weigh 50mL cyclodextrin/hydrophobic and form with pipet
Close polymer solution and the sodium chloride solution that 50mL concentration is 2.00mol/L is positioned in 100mL volumetric flask, be placed on 30 ± 0.05
In DEG C water-bath, after constant temperature, with distilled water diluting to scale, finally shake up.
Further, the concretely comprising the following steps of described step S20:
Step S201, in capillary viscosimeter, add the sample to be tested solution of 10mL, and measure sample to be tested solution
Flow time t1, wherein the mass concentration of this sample to be tested solution is C0；
Step S202, in capillary viscosimeter add 5mL concentration be the sodium chloride solution of 1.00mol/L, sodium chloride is molten
Liquid is mixed homogeneously with the 10mL sample to be tested solution in step S201, then measures the flow time t of mixed solution2, the most now
The concentration of mixed solution is 2/3C0；
Step S203, in capillary viscosimeter, gradually add 5 again, 10,10mL concentration be that the sodium chloride of 1.00mol/L is molten
Liquid, and record flow time t respectively3、t4、t5, wherein the concentration of mixed solution is respectively 1/2C0、1/3C0、1/4C0；
Step S204, by above-mentioned capillary viscosimeter clean dry, add the sodium chloride that 10mL concentration is 1.00mol/L
Solution, constant temperature measures flow time t after 10 minutes0；
Step S205, calculated concentration respectively by following equation be C0、1/2C0、1/3C0、1/4C0The increasing of mixed solution
Specific viscosity ηsp: ηsp=(t-t0)/t
In formula: ηspSpecific viscosity；
The flow time of t solution, s；
t0The flow time of the sodium chloride solution of 1.00mol/L, s；
Step S206, calculate reduced viscosity η of solution the most respectivelysp/C。
Further, the preparation process of described sodium chloride solution is: fix a tool plug conical flask in water bath with thermostatic control,
Add the sodium chloride solution that concentration is 1.00mol/L that dry glass sand core funnel filters, constant temperature 30 minutes wherein.
Further, described capillary viscosity is calculated as Ubbelohde viscometer.
Further, concretely comprising the following steps of described step S30: with mass concentration C as abscissa, reduced viscosity ηsp/ C is
Vertical coordinate does scatterplot, linear regression thickness linear extrapolation to vertical coordinate, the intercept on vertical coordinate, is intrinsic viscosity.
Further, concretely comprising the following steps of described step S40: with the fitting tool in excel, to ηsp/ C～C scatterplot
Figure carries out linear fit, investigates and determines coefficients R2Whether meet R2＞ 0.98；If meeting explanation, heat resistance and salt tolerance is shielded completely
Cover, then stop operation；Otherwise, heat resistance and salt tolerance is shielded the most completely, and the intrinsic viscosity error recorded is relatively big, should improve step
The consumption of rapid S103 cyclodextrin, repetitive operation, until meeting R2During ＞ 0.98.Wherein determine coefficients R2It it is the tolerance goodness of fit
Statistic, the goodness of fit refers to the regression straight line fitting degree to observation.R2Span be between 0 to 1, R2's
Value, closer to 1, illustrates that regression straight line is the best to the fitting degree of observation, otherwise the poorest.
Beneficial effects of the present invention: utilize cyclodextrin to have the feature of hydrophobic cavity, inclusion hydrophobic group, shield hydrophobic forming
Cooperation is used, it is to avoid the supermolecule that association is formed assembles the impact on hydrophobic associated polymer Intrinsic Viscosity Measurements；Measure
Precision is high, can accurately reflect, the unimolecule characteristic of hydrophobic associated polymer；Cyclodextrin does not have surface activity, even if excess is also
Do not interfere with intrinsic viscosity accuracy of measurement, can add excess cyclodextrin method ensure hydrophobic group by complete inclusion, and
Need not the dosage of accurate cyclodextrin, be a kind of characteristic viscosity determining new method being applicable to hydrophobic associated polymer.
Accompanying drawing explanation
Fig. 1 is that in the embodiment of the present invention 1, polymer AP-P4 feature viscosity number measures curve；
Fig. 2 is that in the embodiment of the present invention 2, polymer AP-P4 feature viscosity number measures curve；
Fig. 3 is that in the embodiment of the present invention 3, polymer 3630S feature viscosity number measures curve.
Detailed description of the invention
With embodiment, invention is further described in detail below in conjunction with the accompanying drawings.
A kind of hydrophobic associated polymer Intrinsic Viscosity Measurements method used in embodiment, comprises the following steps:
(1) the solid content S of hydrophobic associated polymer sample, is configured1；
(2), be the hydrophobic association polymer solution of 0.2% with distilled water configuration quality mark, stirring at low speed 2 hours is to dredging
Water association polymer sample is placed 24 hours after being completely dissolved；
(3) cyclodextrin sample solid content S, is weighed2, the hydrophobic associated polymer being added into configuring in step S102 is molten
In liquid, place 2 hours after being completely dissolved, form cyclodextrin/hydrophobic association polymer solution；
(4), accurately weigh 50mL cyclodextrin/hydrophobic association polymer solution with pipet and 50mL concentration is 2.00mol/
The sodium chloride solution of L is positioned in 100mL volumetric flask, is placed in 30 DEG C of water-baths, after constant temperature, with distilled water diluting to scale,
After shake up, be configured to sample to be tested solution；
(5), sample to be tested solution glass core funnel is filtered；
(6), in Ubbelohde viscometer, add the sample to be tested solution of 10mL, and measure the flow time of sample to be tested solution
t1, wherein the mass concentration of this sample to be tested solution is C0；
(7) in water bath with thermostatic control, fix a tool plug conical flask, add what dry glass sand core funnel filtered wherein
Concentration is the sodium chloride solution of 1.00mol/L, constant temperature 30 minutes；
(8), in Ubbelohde viscometer, in addition 5mL (7), concentration is the sodium chloride solution of 1.00mol/L, sodium chloride solution
Mix homogeneously with the 10mL sample to be tested solution in (6), then measure the flow time t of mixed solution2, the most now mixed solution
Concentration be 2/3C0；
(9) in Ubbelohde viscometer, gradually add 5, again, 10,10mL concentration be the sodium chloride solution of 1.00mol/L, and point
Do not record flow time t3、t4、t5, wherein the concentration of mixed solution is respectively 1/2C0,1/3C0、1/4C0；
(10), by above-mentioned Ubbelohde viscometer clean dry, the sodium chloride solution that 10mL concentration is 1.00mol/L is added,
Constant temperature measures flow time t after 10 minutes0；
(11), being calculated concentration respectively by following equation is C0、1/2C0、1/3C0、1/4C0The increasing of mixed solution is than viscous
Degree ηsp: ηsp=(t-t0)/t
In formula: ηspSpecific viscosity；
The flow time of t solution, s；
t0The flow time of the sodium chloride solution of 1.00mol/L, s；
(12) reduced viscosity η of solution, is calculated the most respectivelysp/C；
(13), with mass concentration C as abscissa, reduced viscosity ηsp/ C is that vertical coordinate does scatterplot, and linear regression thickness is straight
Line is extrapolated to vertical coordinate, the intercept on vertical coordinate, is intrinsic viscosity；
(14), with the fitting tool in excel, to ηsp/ C～C scatterplot carry out linear fit, and obtain determining coefficient
R2；
(15) investigation determines coefficients R2Whether meet R2＞ 0.98；If meeting explanation, heat resistance and salt tolerance is shielded completely
Cover, measure the intrinsic viscosity obtained more accurate, stop operation；Otherwise, heat resistance and salt tolerance is shielded the most completely, records
Intrinsic viscosity error is relatively big, should improve the consumption of (3) cyclodextrin, and repetitive operation step (4) is to (14), until meeting R2＞
When 0.98, stopping operation and obtain last intrinsic viscosity, so obtained intrinsic viscosity is the most accurate.
Embodiment 1:
Configuration polymer AP-P4 solution also dilutes, and is diluted to 1000mg/L and 750mg/ containing 1.00mol/L sodium chloride
The polymer solution of L.Design temperature is 30 DEG C, is measured the polymer solution of different initial concentration by determination of ubbelohde viscometer
Flow time, calculates ηsp, then with mass concentration C as abscissa, reduced viscosity ηsp/ C is that vertical coordinate draws ηsp/ C～C scatterplot
Figure.The AP-P4 polymer solution of different initial concentrations is under conditions of being added without cyclodextrin, and the linearity relation of matching is very
Difference, though and the η recorded under the AP-P4 polymer solution same concentrations of different initial concentrationsp/ C also differs, and this explanation is dredged
The intrinsic viscosity that association in water association polymer causes usual manner to record is inaccurate, it is impossible to correctly reflect hydrophobic association
The strand characteristic of polymer.Refer to accompanying drawing 1.
Embodiment 2:
Configuration polymer AP-P4 solution also dilutes, and is diluted to the AP-P4 of 1000mg/L containing 1.00mol/L sodium chloride
Solution, and add the cyclodextrin of 50 times of hydrophobic group molar content, stir.Design temperature is 30 DEG C, by Ubbelohde viscosity
The flow time of the polymer solution of the fixed different initial concentrations of measurement location survey, calculates ηsp, then with mass concentration C as abscissa,
Reduced viscosity ηsp/ C is that vertical coordinate draws ηsp/ C～C scatterplot.AP-P4 polymer solution is adding 50 times of hydrophobic group mole
Under conditions of the cyclodextrin of content, linear fit obtains determining coefficients R2＞ 0.98.The cyclodextrin that hydrophobic association is added into is described
Completely inhibiting, the intrinsic viscosity obtained is accurate, refers to accompanying drawing 2.
Embodiment 3:
Configuration polymer 3630S solution also dilutes, and is diluted to three parts, and every part is all the 1000mg/ of 1.00mol/L sodium chloride
The 3630S solution of L, wherein two parts of cyclodextrin being separately added into 30 and 40 times of hydrophobic group molar content, stir, another part
It is added without cyclodextrin.Design temperature is 30 DEG C, is measured the polymer solution of different initial concentration by determination of ubbelohde viscometer
Flow time, calculates ηsp, then with mass concentration C as abscissa, reduced viscosity ηsp/ C is that vertical coordinate draws ηsp/ C～C scatterplot
Figure.Different rings dextrin adds calculated intrinsic viscosity, does not changes significantly, illustrates that the addition of excess cyclodextrin is right
The intrinsic viscosity of the polyacrylamide solution without hydrophobic group does not affect, and the characteristic of hydrophobic associated polymer is glued by cyclodextrin
The impact of number is derived only from its clathration to hydrophobic group, refers to accompanying drawing 3.
Claims (10)
1. a hydrophobic associated polymer Intrinsic Viscosity Measurements method, it is characterised in that comprise the following steps:
Step S10, preparation hydrophobic association polymer solution, add Cyclodextrin, sodium chloride molten in hydrophobic association polymer solution
Liquid, makes sample to be tested solution；
Step S20, in the sample to be tested solution of hydrophobic associated polymer, add sodium chloride solution, then measure hydrophobic forming respectively
Close sample to be tested solution and mass concentration C of mixed solution, the specific viscosity η of polymersp, reduced viscosity ηsp/C；
Step S30, determine intrinsic viscosity by excel diagram method；
Step S40, estimated performance viscosity number [η] is tested.
A kind of hydrophobic associated polymer Intrinsic Viscosity Measurements method the most according to claim 1, it is characterised in that described step
Rapid S10 concretely comprises the following steps:
Step S101, the solid content S of preparation hydrophobic associated polymer sample1；
Step S102, in hydrophobic associated polymer style add distilled water be configured to hydrophobic association polymer solution；
Step S103, addition cyclodextrin are configured to cyclodextrin/hydrophobic association polymer solution；
Step S104, cyclodextrin/hydrophobic association polymer solution and sodium chloride solution are positioned in 100mL volumetric flask, and use
Distilled water diluting, to scale, is configured to sample to be tested solution；
Step S105, by sample to be tested solution with glass core funnel filter.
A kind of hydrophobic associated polymer Intrinsic Viscosity Measurements method the most according to claim 2, it is characterised in that described step
Rapid S102 is particularly as follows: be the hydrophobic association polymer solution of 0.2% with distilled water preparation mass fraction, and stirring at low speed 2 hours is extremely
Hydrophobic associated polymer sample is placed 24 hours after being completely dissolved.
A kind of hydrophobic associated polymer Intrinsic Viscosity Measurements method the most according to claim 2, it is characterised in that described step
Rapid S103 is particularly as follows: weigh cyclodextrin sample solid content S2, it is added into the hydrophobic associated polymer prepared in step S102
In solution, place 2 hours after being completely dissolved.
A kind of hydrophobic associated polymer Intrinsic Viscosity Measurements method the most according to claim 2, it is characterised in that described step
The step of rapid S104 particularly as follows: accurately weigh 50mL cyclodextrin/hydrophobic association polymer solution and 50mL concentration is with pipet
The sodium chloride solution of 2.00mol/L is positioned in 100mL volumetric flask, is placed in 30 ± 0.05 DEG C of water-baths, after constant temperature, uses distilled water
It is diluted to scale, finally shakes up.
6. according to a kind of hydrophobic associated polymer Intrinsic Viscosity Measurements method described in claim 2 to 5 any one claim,
It is characterized in that, concretely comprising the following steps of described step S20:
Step S201, in capillary viscosimeter, add the sample to be tested solution of 10mL, and measure flowing through of sample to be tested solution
Time t1, wherein the mass concentration of this sample to be tested solution is C0；
Step S202, in capillary viscosimeter add 5mL concentration be the sodium chloride solution of 1.00mol/L, sodium chloride solution with
10mL sample to be tested solution mix homogeneously in step S201, then measure the flow time t of mixed solution2, the most now mix
The concentration of solution is 2/3C0；
Step S203, in capillary viscosimeter, gradually add 5 again, 10,10mL concentration be the sodium chloride solution of 1.00mol/L,
And record flow time t respectively3、t4、t5, wherein the concentration of mixed solution is respectively 1/2C0、1/3C0、1/4C0；
Step S204, by above-mentioned capillary viscosimeter clean dry, add the sodium chloride that 10mL concentration is 1.00mol/L molten
Liquid, constant temperature measures flow time t after 10 minutes0；
Step S205, calculated concentration respectively by following equation be C0、1/2C0、1/3C0、1/4C0The specific viscosity of mixed solution
ηsp: ηsp=(t-t0)/t
In formula: ηspSpecific viscosity；
The flow time of t solution, s；
t0The flow time of the sodium chloride solution of 1.00mol/L, s；
Step S206, calculate reduced viscosity η of solution the most respectivelysp/C。
A kind of hydrophobic associated polymer Intrinsic Viscosity Measurements method the most according to claim 6, it is characterised in that described chlorine
The preparation process changing sodium solution is: fixes a tool plug conical flask in water bath with thermostatic control, adds dry glass core wherein
The sodium chloride solution that concentration is 1.00mol/L that funnel filters, constant temperature 30 minutes.
A kind of hydrophobic associated polymer Intrinsic Viscosity Measurements method the most according to claim 7, it is characterised in that described hair
Capillary viscometer is Ubbelohde viscometer.
A kind of hydrophobic associated polymer Intrinsic Viscosity Measurements method the most according to claim 8, it is characterised in that described step
Rapid S30 concretely comprises the following steps: with mass concentration C as abscissa, reduced viscosity ηsp/ C is that vertical coordinate does scatterplot, and linear regression is thick
Degree linear extrapolation, to vertical coordinate, the intercept on vertical coordinate, is intrinsic viscosity.
A kind of hydrophobic associated polymer Intrinsic Viscosity Measurements method the most according to claim 9, it is characterised in that described
Concretely comprising the following steps of step S40: with the fitting tool in excel, to ηsp/ C～C scatterplot carry out linear fit, and investigation determines
Coefficients R2Whether meet R2＞ 0.98；If meeting explanation, heat resistance and salt tolerance is shielded completely, is then stopped operation；Otherwise, hydrophobic
Association is shielded the most completely, and the intrinsic viscosity error recorded is relatively big, should improve the consumption of cyclodextrin, repetitive operation, directly
To meeting R2During ＞ 0.98.
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