CN106383120A - Method for measuring sulfonation degree of lignosulfonate - Google Patents
Method for measuring sulfonation degree of lignosulfonate Download PDFInfo
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- 238000006277 sulfonation reaction Methods 0.000 title claims abstract description 86
- 229920001732 Lignosulfonate Polymers 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 52
- 238000002835 absorbance Methods 0.000 claims abstract description 62
- 238000000975 co-precipitation Methods 0.000 claims abstract description 19
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000006228 supernatant Substances 0.000 claims description 25
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical group [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 23
- 238000001556 precipitation Methods 0.000 claims description 6
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 3
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 claims 3
- 230000031700 light absorption Effects 0.000 claims 1
- 229920005610 lignin Polymers 0.000 abstract description 21
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000002244 precipitate Substances 0.000 abstract description 4
- 238000007796 conventional method Methods 0.000 abstract description 2
- 125000000524 functional group Chemical group 0.000 abstract description 2
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 abstract 3
- -1 ammonium ions Chemical class 0.000 abstract 1
- 238000013098 chemical test method Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 150
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 63
- 238000000954 titration curve Methods 0.000 description 38
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 36
- 239000011734 sodium Substances 0.000 description 35
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 21
- 229910052708 sodium Inorganic materials 0.000 description 21
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 11
- 239000003456 ion exchange resin Substances 0.000 description 11
- 229920003303 ion-exchange polymer Polymers 0.000 description 11
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 9
- 239000003513 alkali Substances 0.000 description 9
- 239000002023 wood Substances 0.000 description 9
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 8
- 229920001467 poly(styrenesulfonates) Polymers 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 239000004575 stone Substances 0.000 description 8
- 238000004448 titration Methods 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 229940059939 kayexalate Drugs 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 238000002479 acid--base titration Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000011002 quantification Methods 0.000 description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 4
- 238000000108 ultra-filtration Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000003556 assay Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004452 microanalysis Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000004537 pulping Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 229910001626 barium chloride Inorganic materials 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002477 conductometry Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 125000000542 sulfonic acid group Chemical group 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 229920000875 Dissolving pulp Polymers 0.000 description 1
- DYUQAZSOFZSPHD-UHFFFAOYSA-N Phenylpropyl alcohol Natural products CCC(O)C1=CC=CC=C1 DYUQAZSOFZSPHD-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 238000011481 absorbance measurement Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003729 cation exchange resin Substances 0.000 description 1
- 229920001429 chelating resin Polymers 0.000 description 1
- 238000000205 computational method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000003918 potentiometric titration Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/82—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a precipitate or turbidity
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Engineering & Computer Science (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention belongs to the technical field of chemical test method, and discloses a method for measuring the sulfonation degree of lignosulfonate. According to the method, a cetyl trimethyl ammonium bromide (CTAB) co-precipitation method is adopted to measure the sulfonation degree of lignosulfonate. According to the method, CTAB and lignosulfonate are co-precipitated, an ultraviolet spectrophotometer is used to measure the absorbance of lignosulfonate in the supernate, and the sulfonation degree can be calculated through the using amount of CTAB. According to the method, by adjusting the pH of the system to 5.5, the sulfo group of lignin is completely ionized, at the same time, other functional groups are not ionized; then ammonium ions of CTAB react with sulfo groups, charges are neutralized, CTAB and sulfo groups form aggregate and precipitate, and the sulfonation degree can be calculated out by measuring the minimal absorbance and the using amount of CTAB. The provided method has the advantages that the result is similar with that of a conventional method, the method only needs an ultraviolet spectrophotometer or a visible spectrophotometer, the sulfonation degree can be accurately and conveniently measured, and the method is simple and quick.
Description
Technical field
The invention belongs to test chemical method and technology field, particularly to a kind of side measuring lignosulfonates sulfonation degree
Method, specially utilizes the method that cetyl trimethylammonium bromide (CTAB) coprecipitation measures lignosulfonates sulfonation degree.
Background technology
Lignosulfonates are mainly derived from sodium bisulfite pulping waste liquor, neutral sodium sulfite pulping waste liquid, and
The sulfonated products of alkali lignin, connect sulfonic acid group by the side chain of the phenylpropyl alcohol alkyl structure in lignin for the sulfonating reaction, it is not only
Containing a large amount of hydrophobic structures, such as aromatic ring and aliphatic carbon chain, the also hydrophily sense such as sulfonic group, carboxyl, phenolic hydroxyl group simultaneously
Group.The sulfonation degree of lignosulfonates reflects the content of sulfonic acid group in lignosulfonates, is defined as in unit mass (g)
MM content (mmol) of sulfonate radical.Sulfonation degree is the many such as impact lignosulfonates dispersiveness, salt-resistance, surface-active
The principal element of important performance.Therefore effectively measure the sulfonation degree of lignosulfonates, answer for expanding lignosulfonates
With field and its application performance of raising, there is highly important directive significance.However, at present in the world with regard to lignosulfonates
There is larger dispute always in the assay method of sulfonation degree.Existing research shows, the method measuring sulfonation degree at present both at home and abroad
The main inclusion precipitation method, elemental microanalysis method, ion exchange resin and conductometry, acid-base titration.
The method measuring lignosulfonates sulfonation degree at present mainly includes the precipitation method, elemental microanalysis method, amberlite
Fat and conductometry, acid-base titration.But research shows, said method all has some limitations：(1) precipitation method can not
Exclusion water in micro also with BaCl2Ca in the impact of the ion of reaction, such as solution2+, Mg2+, CO3 2-Deng with BaCl2Reaction also can
Produce precipitation, therefore there is larger error.(2) elemental microanalysis method has high demands to analytical equipment, and cost is also higher, and for sulfonation
Spend relatively low lignosulfonates, its sulfur content is relatively low, and elemental analyser cannot its sulfur content of Accurate Determining.(3)
In acid-base titration titration process, acid, the demarcation of alkali concentration of standard solution, the determination influences to the sulfonation degree of lignosulfonates
Larger.Meanwhile, during acid base titration, the error of the judgement of equivalent point, also can affect the accuracy that final sulfonation degree measures.
(4) potentiometric titration is present most common method, but due to titration before sample need to process by anion-cation exchange resin,
Crossing, ion exchange process middle-molecular-weihydroxyethyl is big, and sulfonation degree is relatively low, and water-soluble poor part is trapped within resin, particularly right
The sample obtaining in alkali lignin sulfonation, therefore the sulfonation degree that the method measures is higher, and complex operation, experimental repeatability is poor.
Content of the invention
In order to overcome shortcoming and the deficiency of prior art, the primary and foremost purpose of the present invention is to provide a kind of detecting step simple
Fast, the method that efficiency high and result accurately measure lignosulfonates sulfonation degree, the inventive method is specially and utilizes 16
The method that alkyl trimethyl ammonium bromide (CTAB) coprecipitation measures lignosulfonates sulfonation degree.
The purpose of the present invention is realized by following proposal：
A kind of measure lignosulfonates sulfonation degree method, by using cetyl trimethylammonium bromide (CTAB) with
Lignosulfonates are co-precipitated, and measure the absorbance of supernatant lignosulfonates using ultraviolet specrophotometer, by 16
The consumption of alkyl trimethyl ammonium bromide (CTAB) is calculated sulfonation degree.
The method of said determination lignosulfonates sulfonation degree, specifically includes following steps：
(1) configure lignosulfonate solutions, and adjust pH to 5.5, measure its ultraviolet absorptivity；
(2) it is separately added into a series of CTAB solution of different amounts, constant volume, standing toward lignosulfonate solutions；
(3) mixed liquor centrifugal treating after standing, supernatant measures its ultraviolet absorptivity, when absorbance is minimum, is defined as
Precipitate completely, sulfonation degree is calculated by the consumption of CTAB solution when this.
The inventive method be not subject to temperature, ultrasonically treated etc. affect, described operation all can be carried out at ambient temperature, therefore,
Configuration lignosulfonate solutions etc. can be carried out at room temperature, and need not carry out the operation such as ultrasonically treated, detection method operation letter
Just.
Preferably, described lignosulfonates are sodium lignin sulfonate.
Preferably, described lignosulfonate solutions concentration is 0.5～2g/L.
Preferably, described lignosulfonate solutions concentration is 1g/L.
Preferably, the concentration of described CTAB solution is 0.005～0.02mol/L.
Preferably, the concentration of described CTAB solution is 0.01mol/L.
Preferably, the consumption of described CTAB solution is the 1～40% of lignosulfonate solutions volume.
Preferably, the mensure wavelength of described ultraviolet absorptivity is 280nm.
Preferably, the condition of described centrifugation is 8000～12000rpm centrifugal treating 8～15min.
Preferably, described supernatant can be diluted processing, so that its range of absorbency falls in purple before mensuration absorbance
Measurement range can obtain final result it is ensured that the accuracy of absorbance, then by the multiple conversion of dilution outward.
The present invention adopts ultraviolet specrophotometer to measure the absorbance of the lignosulfonates of residual in supernatant, works as extinction
When degree is minimum it is believed that now sulfonic group neutralized completely by ammonium ion, sulfonation degree can be calculated by the consumption of CTAB.
When the ionic strength of supernatant after centrifugal treating is larger, the titration curve second half section occurs platform, now processes
Method is：Will appear from the numerical point before platform and be fitted in alignment, the numerical point of platform phase is fitted to one simultaneously
Bar straight line, the intersection point of two lines is the sulfonation degree of sample.
Described sulfonation degree computational methods are as follows：
Note CTAB solution concentration is CCTAB(mol/L) when, absorbance is minimum, corresponding CTAB consumption is VCTAB(L), lignin
Sulfonate concentration is CSL(g/L), lignosulfonates sampling amount is VSL(L), corresponding computing formula is：
The pH that the inventive method adjusts lignosulfonates first be 5.5 so as in sulfonic group ionize completely, and other
Functional group's unionization, adds CTAB, with sulfonic group in lignosulfonates, charging neutrality occurs using the ammonium ion in CTAB
Effect, lignosulfonates form aggregation in the solution and precipitate.By mensuration absorbance, when absorbance is minimum,
Think that now sulfonic group is fully neutralized, sulfonation degree can be calculated by the consumption of CTAB.The sulfonation degree that the method measures
Preferably, instrument needed for mensure is only ultraviolet or visible spectrophotometer to the sulfonation degree result goodness of fit measuring with conventional method, is
The Accurate Determining of sulfonation degree brings facility, has the advantages that simple and fast.
The present invention, with respect to prior art, has such advantages as and beneficial effect：
(1) detecting instrument needed for the present invention measures sulfonation degree is only ultraviolet-visible spectrophotometer, required main examination
Agent is only CTAB, overcomes the limitation of traditional assay method, has the cheap advantage of testing cost.
(2) process before the present invention does not need sample is carried out when measuring, simple and quick.
(3) measurement result of the present invention is accurate, favorable reproducibility.
Brief description
Fig. 1 is temperature, the impact figure to assay method of the present invention for the condition such as ultrasonic, comprises embodiment 1, embodiment 2 is implemented
Example 3.
Fig. 2 measures the sulfonation degree titration curve of SKL-1 for CTAB coprecipitation.
Fig. 3 measures the sulfonation degree titration curve of SKL-2 for CTAB coprecipitation.
Fig. 4 measures the sulfonation degree titration curve of SKL-3 for CTAB coprecipitation.
Fig. 5 is that elementary analysis, constant-current titration and CTAB coprecipitation measure stone Xian wood sodium, SL-1, SL-2, SL-3 and SL-4
Sulfonation degree result comparison diagram, comprise embodiment 1, embodiment 10, embodiment 11, embodiment 12 and embodiment 13.
Fig. 6 is elementary analysis, constant-current titration and CTAB coprecipitation measure the wooden sodium of purification, SKL-1, SKL-2, SKL-3,
The comparison diagram of the sulfonation degree result of SMN-1, SMN-2 and SMN-3, comprises embodiment 4, embodiment 5, embodiment 6, embodiment 7, reality
Apply example 8 and embodiment 9.
Fig. 7 be ionic strength to CTAB coprecipitation measure sulfonation degree impact figure, comprise embodiment 14, embodiment 15,
Embodiment 16 and embodiment 17.
Fig. 8 is the graph of a relation of the absorbance with PSS compound for the different proportion CTAB and surface charge.
Specific embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention do not limit
In this.
In the following example, agents useful for same all can be commercially available from market, the dissimilar lignosulfonates in embodiment
Preparation method is as follows：
The preparation of the sulfomethylation product (SKL) of alkali lignin：Raw material is industrial alkali lignin, by city of Hunan Huaihua along safe
Science and Technology Ltd. provides, and is pine alkaline process dissolving pulp black liquor acid out gained.The sodium lignin sulfonate of different sulfonation degree pass through with
Lower section method prepares：Industrial alkali lignin is added in the sodium hydroxide solution of 1mol/L, 1h is stirred at room temperature, by solution plus
Heat, to after 75 DEG C, adds formalin, after mixing 1h, is warming up to 95 DEG C, and being separately added into mass fraction is 20%, 30%, 40%
Na2SO3Reaction 4h, obtains sample SKL-1, SKL-2, SKL-3 by purification.
The preparation of the sulfomethylation product (SMN) of alkali lignin：Weigh alkali lignin (passage paper mill) 100g, it contains admittedly
Measure as 22.7%, initial pH is 10.16, is heated to 73 DEG C, add the formaldehyde of 2mmol/g, 4mmol/g, 6mmol/g, insulation
1.5h, is warming up to 90 DEG C, adds Na2SO3(n (formaldehyde)：n(Na2SO3)=1：1.1), being concentrated by evaporation to solid content is 30%, protects
Warm 8h, obtains sample SMN-1, SMN-2, SMN-3 by purification.
The ultrafiltration classification of sodium lignin sulfonate：By unpurified sodium lignin sulfonate be configured to mass fraction be 10% molten
Liquid, after stirring makes it be completely dissolved, removes insoluble matter therein by suction filtration.Reuse UF201 ultrafilter to lignin sulfonic acid
Sodium solution carries out ultrafiltration processing.In experiment the retention weight average molecular weight of milipore filter used be respectively 2500Da, 10
000Da and 50 000Da.First the sodium lignin sulfonate treating suction filtration is passed through the milipore filter that molecular weight is 50000Da, you can super
Filter obtains molecular weight and is more than the ultrafiltrate that 50000Da and molecular weight are less than 50000Da；Again molecular weight is less than the super of 50000Da
Filtrate is the milipore filter of 10000Da by molecular cut off, you can it is 10000～50000Da and molecule that ultrafiltration obtains molecular weight
The ultrafiltrate less than 10000Da for the amount；The ultrafiltrate that molecular weight is finally less than 10000Da is 2500Da's by molecular cut off
Milipore filter, you can ultrafiltration obtains ultrafiltrate that molecular weight is 2500～110000Da and molecular weight is less than the ultrafiltrate of 2500Da.
Molecular weight be can get by above-mentioned flow process and be greater than 50 000Da, 10 000Da～50 000Da, 2500Da～10 respectively
000Da, four different fractions less than 2500Da, are respectively labeled as SL1, SL2, SL3, SL4.Wood by aforementioned four fraction
Quality sodium sulfonate solution revolving, dries, and grinds, is placed in standby in drier.
Embodiment 1
By the sodium lignin sulfonate of ultraviolet specrophotometer quantitative configuration 1g/L (stone Xian wood sodium, SL) solution, respectively to
Wherein drip the hydrochloric acid solution of a small amount of 0.1mol/L and 0.1mol/L sodium hydroxide solution to adjust lignin sulfonic acid sodium solution
PH, the pH making system is 5.5, and stands 1h at room temperature.Configure the CTAB solution of 0.01mol/L simultaneously.Accurately pipette 10mL
, in the volumetric flask of 25mL, the CTAB sequentially adding 0.5～2.5mL (volume is spaced apart 0.1mL) is molten for lignin sulfonic acid sodium solution
Liquid, in volumetric flask, shakes up standing 10min, takes 1.5mL mixed liquor in centrifuge tube, and 10000rpm centrifugal treating 10min takes
1mL supernatant dilutes, and is measured using ultraviolet specrophotometer, by absorbance at 280nm for the absorbance curve and CTAB
Consumption determine a titration curve.
Embodiment 2
By the sodium lignin sulfonate of ultraviolet specrophotometer quantitative configuration 1g/L (stone Xian wood sodium, SL) solution, respectively to
Wherein drip the hydrochloric acid solution of a small amount of 0.1mol/L and 0.1mol/L sodium hydroxide solution to adjust lignin sulfonic acid sodium solution
PH, the pH making system is 5.5, and stands 1h at 50 DEG C.Configure the CTAB solution of 0.01mol/L simultaneously.Accurately pipette 10mL
, in the volumetric flask of 25mL, the CTAB sequentially adding 0.5～2.5mL (volume is spaced apart 0.1mL) is molten for lignin sulfonic acid sodium solution
Liquid, in volumetric flask, shakes up standing 10min, takes 1.5mL mixed liquor in centrifuge tube, and 10000rpm centrifugal treating 10min takes
1mL supernatant dilutes, and is measured using ultraviolet specrophotometer, by absorbance at 280nm for the absorbance curve and CTAB
Consumption determine a titration curve.
Embodiment 3
By the sodium lignin sulfonate of ultraviolet specrophotometer quantitative configuration 1g/L (stone Xian wood sodium, SL) solution, respectively to
Wherein drip the hydrochloric acid solution of a small amount of 0.1mol/L and 0.1mol/L sodium hydroxide solution to adjust lignin sulfonic acid sodium solution
PH, the pH making system is 5.5, and stands 1h at 20 DEG C, and ultrasonic 30min.Configure the CTAB solution of 0.01mol/L simultaneously.
Accurately pipette 10mL lignin sulfonic acid sodium solution in the volumetric flask of 25mL, (volume is spaced apart to sequentially add 0.5～2.5mL
CTAB solution 0.1mL), in volumetric flask, shakes up standing 10min, takes 1.5mL mixed liquor in centrifuge tube, 10000rpm is centrifuged
Process 10min, take 1mL supernatant to dilute, be measured using ultraviolet specrophotometer, by absorbance curve at 280nm
Absorbance determines a titration curve with the consumption of CTAB.
Embodiment 4
By the SKL-1 solution of ultraviolet specrophotometer quantitative configuration 1g/L, drip a small amount of 0.1mol/L respectively thereto
Hydrochloric acid solution and 0.1mol/L sodium hydroxide solution adjusting the pH of SKL-1 solution, the pH making system is 5.5.Configure simultaneously
The CTAB solution of 0.01mol/L.Accurately pipette 10mL SKL-1 solution in the volumetric flask of 25mL, sequentially add 0.5～2.5mL
The CTAB solution of (volume is spaced apart 0.1mL), in volumetric flask, shakes up standing 10min, takes 1.5mL mixed liquor in centrifuge tube,
10000rpm centrifugal treating 10min, is taken 1mL supernatant to dilute, is measured using ultraviolet specrophotometer, by absorbance curve
Absorbance at 280nm determines a titration curve with the consumption of CTAB, corresponding CTAB when absorbance is minimum in titration curve
Consumption be the sulfonation degree of this sample.
Embodiment 5
By the SKL-2 solution of ultraviolet specrophotometer quantitative configuration 1g/L, drip a small amount of 0.1mol/L respectively thereto
Hydrochloric acid solution and 0.1mol/L sodium hydroxide solution adjusting the pH of SKL-2 solution, the pH making system is 5.5.Configure simultaneously
The CTAB solution of 0.01mol/L.Accurately pipette 10mL SKL-2 in the volumetric flask of 25mL, sequentially add 0.5～2.5mL (body
Long-pending be spaced apart 0.1mL) CTAB solution in volumetric flask, shake up standing 10min, take 1.5mL mixed liquor in centrifuge tube,
10000rpm centrifugal treating 10min, is taken 1mL supernatant to dilute, is measured using ultraviolet specrophotometer, by absorbance curve
Absorbance at 280nm determines a titration curve with the consumption of CTAB, corresponding CTAB when absorbance is minimum in titration curve
Consumption be the sulfonation degree of this sample.
Embodiment 6
By the SKL-3 solution of ultraviolet specrophotometer quantitative configuration 1g/L, drip a small amount of 0.1mol/L respectively thereto
Hydrochloric acid solution and 0.1mol/L sodium hydroxide solution adjusting the pH of SKL-3 solution, the pH making system is 5.5.Configure simultaneously
The CTAB solution of 0.01mol/L.Accurately pipette 10mL SKL-3 solution in the volumetric flask of 25mL, sequentially add 0.5～2.5mL
The CTAB solution of (volume is spaced apart 0.1mL), in volumetric flask, shakes up standing 10min, takes 1.5mL mixed liquor in centrifuge tube,
10000rpm centrifugal treating 10min, is taken 1mL supernatant to dilute, is measured using ultraviolet specrophotometer, by absorbance curve
Absorbance at 280nm determines a titration curve with the consumption of CTAB, corresponding CTAB when absorbance is minimum in titration curve
Consumption be the sulfonation degree of this sample.
Embodiment 7
By the SMN-1 solution of ultraviolet specrophotometer quantitative configuration 1g/L, drip a small amount of 0.1mol/L respectively thereto
Hydrochloric acid solution and 0.1mol/L sodium hydroxide solution adjusting the pH of SMN-1 solution, the pH making system is 5.5.Configure simultaneously
The CTAB solution of 0.01mol/L.Accurately pipette 10mL SMN-1 solution in the volumetric flask of 25mL, sequentially add 0.5～2.5mL
The CTAB solution of (volume is spaced apart 0.1mL), in volumetric flask, shakes up standing 10min, takes 1.5mL mixed liquor in centrifuge tube,
10000rpm centrifugal treating 10min, is taken 1mL supernatant to dilute, is measured using ultraviolet specrophotometer, by absorbance curve
Absorbance at 280nm determines a titration curve with the consumption of CTAB, corresponding CTAB when absorbance is minimum in titration curve
Consumption be the sulfonation degree of this sample.
Embodiment 8
By the SMN-2 solution of ultraviolet specrophotometer quantitative configuration 1g/L, drip a small amount of 0.1mol/L respectively thereto
Hydrochloric acid solution and 0.1mol/L sodium hydroxide solution adjusting the pH of SMN-2 solution, the pH making system is 5.5.Configure simultaneously
The CTAB solution of 0.01mol/L.Accurately pipette 10mL SMN-2 solution in the volumetric flask of 25mL, sequentially add 0.5～2.5mL
The CTAB solution of (volume is spaced apart 0.1mL), in volumetric flask, shakes up standing 10min, takes 1.5mL mixed liquor in centrifuge tube,
10000rpm centrifugal treating 10min, is taken 1mL supernatant to dilute, is measured using ultraviolet specrophotometer, by absorbance curve
Absorbance at 280nm determines a titration curve with the consumption of CTAB, corresponding CTAB when absorbance is minimum in titration curve
Consumption be the sulfonation degree of this sample.
Embodiment 9
By the SMN-3 solution of ultraviolet specrophotometer quantitative configuration 1g/L, drip a small amount of 0.1mol/L respectively thereto
Hydrochloric acid solution and 0.1mol/L sodium hydroxide solution adjusting the pH of SMN-3 solution, the pH making system is 5.5.Configure simultaneously
The CTAB solution of 0.01mol/L.Accurately pipette 10mL SMN-3 solution in the volumetric flask of 25mL, sequentially add 0.5～2.5mL
The CTAB solution of (volume is spaced apart 0.1mL), in volumetric flask, shakes up standing 10min, takes 1.5mL mixed liquor in centrifuge tube,
10000rpm centrifugal treating 10min, is taken 1mL supernatant to dilute, is measured using ultraviolet specrophotometer, by absorbance curve
Absorbance at 280nm determines a titration curve with the consumption of CTAB, corresponding CTAB when absorbance is minimum in titration curve
Consumption be the sulfonation degree of this sample.
Embodiment 10
By the SL-1 solution of ultraviolet specrophotometer quantitative configuration 1g/L, drip a small amount of 0.1mol/L's respectively thereto
Adjusting the pH of SL-1 solution, the pH making system is 5.5 for hydrochloric acid solution and 0.1mol/L sodium hydroxide solution.Configure simultaneously
The CTAB solution of 0.01mol/L.Accurately pipette 10mL SL-1 solution in the volumetric flask of 25mL, sequentially add 0.5～2.5mL
The CTAB solution of (volume is spaced apart 0.1mL), in volumetric flask, shakes up standing 10min, takes 1.5mL mixed liquor in centrifuge tube,
10000rpm centrifugal treating 10min, is taken 1mL supernatant to dilute, is measured using ultraviolet specrophotometer, by absorbance curve
Absorbance at 280nm determines a titration curve with the consumption of CTAB, corresponding CTAB when absorbance is minimum in titration curve
Consumption be the sulfonation degree of this sample.
Embodiment 11
By the SL-2 solution of ultraviolet specrophotometer quantitative configuration 1g/L, drip a small amount of 0.1mol/L's respectively thereto
Adjusting the pH of SL-2 solution, the pH making system is 5.5 for hydrochloric acid solution and 0.1mol/L sodium hydroxide solution.Configure simultaneously
The CTAB solution of 0.01mol/L.Accurately pipette 10mL SL-2 solution in the volumetric flask of 25mL, sequentially add 0.5～2.5mL
The CTAB solution of (volume is spaced apart 0.1mL), in volumetric flask, shakes up standing 10min, takes 1.5mL mixed liquor in centrifuge tube,
10000rpm centrifugal treating 10min, is taken 1mL supernatant to dilute, is measured using ultraviolet specrophotometer, by absorbance curve
Absorbance at 280nm determines a titration curve with the consumption of CTAB, corresponding CTAB when absorbance is minimum in titration curve
Consumption be the sulfonation degree of this sample.
Embodiment 12
By the SL-3 solution of ultraviolet specrophotometer quantitative configuration 1g/L, drip a small amount of 0.1mol/L's respectively thereto
Adjusting the pH of SL-3 solution, the pH making system is 5.5 for hydrochloric acid solution and 0.1mol/L sodium hydroxide solution.Configure simultaneously
The CTAB solution of 0.01mol/L.Accurately pipette 10mL SL-3 solution in the volumetric flask of 25mL, sequentially add 0.5～2.5mL
The CTAB solution of (volume is spaced apart 0.1mL), in volumetric flask, shakes up standing 10min, takes 1.5mL mixed liquor in centrifuge tube,
10000rpm centrifugal treating 10min, is taken 1mL supernatant to dilute, is measured using ultraviolet specrophotometer, by absorbance curve
Absorbance at 280nm determines a titration curve with the consumption of CTAB, corresponding CTAB when absorbance is minimum in titration curve
Consumption be the sulfonation degree of this sample.
Embodiment 13
By the SL-4 solution of ultraviolet specrophotometer quantitative configuration 1g/L, drip a small amount of 0.1mol/L's respectively thereto
Adjusting the pH of SL-4 solution, the pH making system is 5.5 for hydrochloric acid solution and 0.1mol/L sodium hydroxide solution.Configure simultaneously
The CTAB solution of 0.01mol/L.Accurately pipette 10mL SL-4 solution in the volumetric flask of 25mL, sequentially add 0.5～2.5mL
The CTAB solution of (volume is spaced apart 0.1mL), in volumetric flask, shakes up standing 10min, takes 1.5mL mixed liquor in centrifuge tube,
10000rpm centrifugal treating 10min, is taken 1mL supernatant to dilute, is measured using ultraviolet specrophotometer, by absorbance curve
Absorbance at 280nm determines a titration curve with the consumption of CTAB, corresponding CTAB when absorbance is minimum in titration curve
Consumption be the sulfonation degree of this sample.
Embodiment 14
Ion exchange resin treatment is carried out to sodium lignin sulfonate, to remove Na therein2SO3Deng impurity.Divided by ultraviolet
Sodium lignin sulfonate (stone Xian wood sodium, SL) solution after the ion exchange resin treatment of light photometric quantification configuration 1g/L, respectively
Drip the hydrochloric acid solution of a small amount of 0.1mol/L and 0.1mol/L sodium hydroxide solution thereto to adjust the pH of SL solution, make system
PH be 5.5.Configure the CTAB solution of 0.01mol/L simultaneously.Accurately pipette 10mL SL solution in the volumetric flask of 25mL, according to
The CTAB solution of secondary addition 0.5～2.5mL (volume is spaced apart 0.1mL), in volumetric flask, shakes up standing 10min, takes 1.5mL to mix
Close liquid in centrifuge tube, 10000rpm centrifugal treating 10min, take 1mL supernatant to dilute, surveyed using ultraviolet specrophotometer
Fixed, the consumption of absorbance at 280nm for the absorbance curve and CTAB is determined a titration curve.
Embodiment 15
Ion exchange resin treatment is carried out to sodium lignin sulfonate, to remove Na therein2SO3Deng impurity.Divided by ultraviolet
Sodium lignin sulfonate (stone Xian wood sodium, SL) solution after the ion exchange resin treatment of light photometric quantification configuration 1g/L, simultaneously
Mass fraction is added to be respectively the Na of 5% (with respect to the quality of sodium lignin sulfonate) in solution2SO3, drip thereto respectively
Adjusting the pH of SL solution, the pH making system is 5.5 for the hydrochloric acid solution of a small amount of 0.1mol/L and 0.1mol/L sodium hydroxide solution.
Configure the CTAB solution of 0.01mol/L simultaneously.Accurately pipette 10mL SL solution in the volumetric flask of 25mL, sequentially add 0.5～
The CTAB solution of 2.5mL (volume is spaced apart 0.1mL), in volumetric flask, shakes up standing 10min, takes 1.5mL mixed liquor in centrifugation
Guan Zhong, 10000rpm centrifugal treating 10min, is taken 1mL supernatant to dilute, is measured using ultraviolet specrophotometer, by extinction
Absorbance at 280nm for the line of writing music determines a titration curve with the consumption of CTAB.
Embodiment 16
Ion exchange resin treatment is carried out to sodium lignin sulfonate, to remove Na therein2SO3Deng impurity.Divided by ultraviolet
Sodium lignin sulfonate (stone Xian wood sodium, SL) solution after the ion exchange resin treatment of light photometric quantification configuration 1g/L, simultaneously
Mass fraction is added to be respectively the Na of 10% (with respect to the quality of sodium lignin sulfonate) in solution2SO3, drip thereto respectively
Plus the hydrochloric acid solution of a small amount of 0.1mol/L and 0.1mol/L sodium hydroxide solution are adjusting the pH of SL solution, the pH of system is made to be
5.5.Configure the CTAB solution of 0.01mol/L simultaneously.Accurately pipette 10mL SL solution in the volumetric flask of 25mL, sequentially add
The CTAB solution of 0.5～2.5mL (volume is spaced apart 0.1mL) in volumetric flask, shake up standing 10min, take 1.5mL mixed liquor in
In centrifuge tube, 10000rpm centrifugal treating 10min, take 1mL supernatant to dilute, be measured using ultraviolet specrophotometer, will
Absorbance at 280nm for the absorbance curve determines a titration curve with the consumption of CTAB.
Embodiment 17
Ion exchange resin treatment is carried out to sodium lignin sulfonate, to remove Na therein2SO3Deng impurity.Divided by ultraviolet
Sodium lignin sulfonate (stone Xian wood sodium, SL) solution after the ion exchange resin treatment of light photometric quantification configuration 1g/L, simultaneously
Mass fraction is added to be respectively the Na of 20% (with respect to the quality of sodium lignin sulfonate) in solution2SO3, drip thereto respectively
Plus the hydrochloric acid solution of a small amount of 0.1mol/L and 0.1mol/L sodium hydroxide solution are adjusting the pH of SL solution, the pH of system is made to be
5.5.Configure the CTAB solution of 0.01mol/L simultaneously.Accurately pipette 10mL SL solution in the volumetric flask of 25mL, sequentially add
The CTAB solution of 0.5～2.5mL (volume is spaced apart 0.1mL) in volumetric flask, shake up standing 10min, take 1.5mL mixed liquor in
In centrifuge tube, 10000rpm centrifugal treating 10min, take 1mL supernatant to dilute, be measured using ultraviolet specrophotometer, will
Absorbance at 280nm for the absorbance curve determines a titration curve with the consumption of CTAB.
Embodiment 18
Configuration concentration is kayexalate (PSS, molecular weight the is 70000) solution of 1g/L, by dripping thereto
The pH of the hydrochloric acid solution of a small amount of 0.1mol/L and 0.1mol/L sodium hydroxide solution regulation solution is 5.5, configures simultaneously
The CTAB solution of 0.01mol/L.Accurately pipette 10mL SL solution in the volumetric flask of 25mL, sequentially add 0.5～2.5mL (body
Long-pending be spaced apart 0.1mL) CTAB solution in volumetric flask, shake up standing 10min, take 1.5mL mixed liquor in centrifuge tube,
10000rpm centrifugal treating 10min, is taken 1mL supernatant to dilute, is measured using ultraviolet specrophotometer, by absorbance curve
Absorbance at 280nm determines a titration curve with the consumption of CTAB.Carry out with the sulfonation degree of determination of elemental analysis simultaneously
Contrast.And when different CTAB addition is measured by surface charge instrument, the surface of kayexalate and CTAB mixed solution
Electric charge, and the relation of titration curve and surface charge is associated.
In addition to above example, the present invention utilizes SL, SL- in elementary analysis and potentiometric determination embodiment simultaneously
1st, the sulfonation degree of the sample such as SL-2, SL-3, SL-4, SKL-1, SKL-2, SKL-3, SMN-1, SMN-2, SMN-3, with embodiment institute
Survey sulfonation degree to be contrasted.
Fig. 1 (comprising embodiment 1, embodiment 2 and embodiment 3) is that temperature, the different condition such as ultrasonic measure to sulfonation degree
Impact.As shown in Figure 1, under conditions of for difference, bent by the titration of CTAB Precipitation Determination sodium lignin sulfonate sulfonation degree
The rule of line is consistent, and all increases with CTAB addition of its absorbance at 280nm present and first reduce the trend increasing afterwards,
And all when CTAB consumption is 1.5mL, absorbance is minimum, the now corresponding sulfonation degree being this sodium lignin sulfonate.In difference
Under the conditions of, the repeatability of three titration curves preferably, that is, shows, the factor such as temperature, ultrasound condition measures to CTAB coprecipitation
The sulfonation degree of lignosulfonates no affects.
Fig. 2 (embodiment 4), Fig. 3 (embodiment 5) and Fig. 4 (embodiment 6) are the sulphur that CTAB coprecipitation measures SKL series
Change degree titration curve.As seen from the figure, for partial lignin sulfonate sample, measure its sulfonation degree using CTAB coprecipitation
A platform occurs, in order to obtain the exact value of the sulfonation degree of sample, the present invention is to this situation during titration curve
When processing method as follows：Will appear from the numerical point before platform be fitted in alignment, simultaneously by the numerical value of platform phase
Point matching is in alignment, and the intersection point of two lines is the sulfonation degree of sample.
Fig. 5 (comprising embodiment 1, embodiment 10, embodiment 11, embodiment 12 and embodiment 13) and Fig. 6 (comprises embodiment
4th, embodiment 5, embodiment 6, embodiment 7, embodiment 8 and embodiment 9) it is elementary analysis, constant-current titration and CTAB coprecipitation
Measure the contrast of sulfonation degree result.As seen from the figure, the sulfonated products for sodium bisulfite pulping waste liquor and alkali lignin
Sulfonated products, measure sulfonation degree by CTAB coprecipitation less with the sulfonation degree difference of elementary analysis and constant-current titration mensure；
And the repeated preferable of sulfonation degree is measured by CTAB coprecipitation, deviation is less.
Fig. 7 (comprising embodiment 14, embodiment 15, embodiment 16 and embodiment 17) is ionic strength to CTAB coprecipitation
Measure the impact of sulfonation degree, be the analysis further to the phenomenon that platform occurs in Fig. 2, Fig. 3 and Fig. 4.Due to lignin sulfonic acid
The source of sodium is mainly passed through to add Na2SO3Carry out sulfonation with NaOH to lignin to prepare, but sulfomethylated lignin in embodiment
The pH of acid sodium solution is all adjusted to 5.5, therefore in titration process, ignoring the impact of NaOH in solution, platform occurs
Reason is because in solution remaining Na2SO3Impact.As shown in Figure 7, for the lignin sulfonic acid after ion exchange resin treatment
The no obvious platform of the titration curve of sodium, the sulfonation degree of mensure is 1.60；For addition Na2SO3Sample, all occur significantly
Platform, and with Na2SO3The increase of addition, the lasting span of platform is bigger.By to addition Na2SO3Sample titration
Curve is fitted, and the sulfonation degree of mensure is 1.68, with ion exchange resin treatment after sodium lignin sulfonate sulfonation degree
Difference is less, it follows that during CTAB coprecipitation measures lignosulfonates sulfonation degree, the platform of appearance is because
Na2SO3Impact.And prove that the present invention has reliability to the processing method occurring during platform.
Fig. 8 (embodiment 18) is the relation of the absorbance with PSS compound for the different proportion CTAB and surface charge.By Fig. 8
Understand, with the increase of CTAB addition, the absorbance of kayexalate solution assumes the trend of first increases and then decreases, and
Middle a platform, is 3.81mmol/g by the sulfonation degree that CTAB coprecipitation records, and by determination of elemental analysis
Sulfonation degree 3.87mmol/g close.Meanwhile, with the increase of CTAB addition, the surface charge of kayexalate solution
It is gradually increased on the occasion of when CTAB addition is 3.85, the surface charge of solution is approximately zero from negative value.This result shows,
When the sulfonic group in the ammonium ion in CTAB and kayexalate is according to 1:When 1 ratio neutralizes completely, polystyrene sulphur
Sour sodium precipitates completely, and the absorbance of mixed solution is minimum.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not subject to above-described embodiment
Limit, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplify,
All should be equivalent substitute mode, be included within protection scope of the present invention.
Claims (10)
1. a kind of method measuring lignosulfonates sulfonation degree is it is characterised in that by using cetyl trimethylammonium bromide
With lignosulfonates co-precipitation, measure the absorbance of supernatant lignosulfonates using ultraviolet specrophotometer, by ten
The consumption of six alkyl trimethyl ammonium bromides is calculated sulfonation degree.
2. the method measuring lignosulfonates sulfonation degree according to claim 1 is it is characterised in that specifically include following
Step：
(1) configure lignosulfonate solutions, and adjust pH to 5.5, measure its ultraviolet absorptivity；
(2) it is separately added into a series of cetyl trimethylammonium bromide solution of different amounts toward lignosulfonate solutions, fixed
Hold, standing；
(3) mixed liquor centrifugal treating after standing, supernatant measures its ultraviolet absorptivity, when absorbance is minimum, is defined as completely
Precipitation, is calculated sulfonation degree by the consumption of cetyl trimethylammonium bromide solution when this.
3. according to claim 2 measure lignosulfonates sulfonation degree method it is characterised in that：Described lignin
Sulfonate is sodium lignin sulfonate.
4. according to claim 2 measure lignosulfonates sulfonation degree method it is characterised in that：Described lignin
Sulfonate solution concentration is 0.5～2g/L.
5. according to claim 2 measure lignosulfonates sulfonation degree method it is characterised in that：Described lignin
Sulfonate solution concentration is 1g/L.
6. according to claim 2 measure lignosulfonates sulfonation degree method it is characterised in that：Described cetyl
The concentration of trimethylammonium bromide solution is 0.005～0.02mol/L.
7. according to claim 2 measure lignosulfonates sulfonation degree method it is characterised in that：Described cetyl
The concentration of trimethylammonium bromide solution is 0.01mol/L.
8. according to claim 2 measure lignosulfonates sulfonation degree method it is characterised in that：Described cetyl
The consumption of trimethylammonium bromide solution is the 1～40% of lignosulfonate solutions volume.
9. according to claim 2 measure lignosulfonates sulfonation degree method it is characterised in that：Described ultraviolet light absorption
The mensure wavelength of degree is 280nm.
10. according to claim 2 measure lignosulfonates sulfonation degree method it is characterised in that：Described centrifugation
Condition is 8000～12000rpm centrifugal treating 8～15min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107664618A (en) * | 2017-07-20 | 2018-02-06 | 山东金科力电源科技有限公司 | The method of testing of lignosulphonic acid sodium content in lead-acid accumulator green plate |
| CN109709261A (en) * | 2018-11-22 | 2019-05-03 | 中国石油天然气股份有限公司 | Method and instrument for measuring degree of hydrolysis of sulfonate-containing polyacrylamide polymer |
| CN110333199A (en) * | 2019-06-17 | 2019-10-15 | 华南理工大学 | Measuring method of the lignin content to black liquor pollution during a kind of biomass delignification |
| CN111139082A (en) * | 2020-01-14 | 2020-05-12 | 浙江丰瑜生态科技股份有限公司 | Micro-powder soil conditioner and preparation method thereof |
| CN112945953A (en) * | 2021-02-05 | 2021-06-11 | 南京工业大学 | Flow path system of continuous flow turbidimeter |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101571522A (en) * | 2009-06-10 | 2009-11-04 | 谱尼测试科技（北京）有限公司 | Method for measuring content of taurine in food |
| CN101666743A (en) * | 2008-09-05 | 2010-03-10 | 烟台安德利果胶有限公司 | Method for measuring nitrate in pectin |
| WO2011124945A1 (en) * | 2010-04-07 | 2011-10-13 | Empire Technology Development Llc. | Detector for detecting contaminants in water or aqueous solutions |
-
2016
- 2016-08-30 CN CN201610771787.0A patent/CN106383120A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101666743A (en) * | 2008-09-05 | 2010-03-10 | 烟台安德利果胶有限公司 | Method for measuring nitrate in pectin |
| CN101571522A (en) * | 2009-06-10 | 2009-11-04 | 谱尼测试科技（北京）有限公司 | Method for measuring content of taurine in food |
| WO2011124945A1 (en) * | 2010-04-07 | 2011-10-13 | Empire Technology Development Llc. | Detector for detecting contaminants in water or aqueous solutions |
Non-Patent Citations (1)
| Title |
|---|
| 祝都明: "木质素磺酸钠在制备水相石墨烯中的应用及其磺化度的测定", 《学术天下网》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107664618A (en) * | 2017-07-20 | 2018-02-06 | 山东金科力电源科技有限公司 | The method of testing of lignosulphonic acid sodium content in lead-acid accumulator green plate |
| CN109709261A (en) * | 2018-11-22 | 2019-05-03 | 中国石油天然气股份有限公司 | Method and instrument for measuring degree of hydrolysis of sulfonate-containing polyacrylamide polymer |
| CN109709261B (en) * | 2018-11-22 | 2022-02-01 | 中国石油天然气股份有限公司 | Method and instrument for measuring degree of hydrolysis of sulfonate-containing polyacrylamide polymer |
| CN110333199A (en) * | 2019-06-17 | 2019-10-15 | 华南理工大学 | Measuring method of the lignin content to black liquor pollution during a kind of biomass delignification |
| CN111139082A (en) * | 2020-01-14 | 2020-05-12 | 浙江丰瑜生态科技股份有限公司 | Micro-powder soil conditioner and preparation method thereof |
| CN111139082B (en) * | 2020-01-14 | 2021-04-02 | 浙江丰瑜生态科技股份有限公司 | Micro-powder soil conditioner and preparation method thereof |
| CN112945953A (en) * | 2021-02-05 | 2021-06-11 | 南京工业大学 | Flow path system of continuous flow turbidimeter |
| CN112945953B (en) * | 2021-02-05 | 2024-03-01 | 南京工业大学 | Flow path system of continuous flow turbidimetry analyzer |
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Application publication date: 20170208 |