CN108872118B - Method for detecting lignin content of papermaking pre-cooking liquid - Google Patents
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- 229920005610 lignin Polymers 0.000 title claims abstract description 116
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000010411 cooking Methods 0.000 title claims abstract description 20
- 239000007788 liquid Substances 0.000 title claims abstract description 12
- 238000002835 absorbance Methods 0.000 claims abstract description 23
- 238000001514 detection method Methods 0.000 claims abstract description 17
- FXXACINHVKSMDR-UHFFFAOYSA-N acetyl bromide Chemical compound CC(Br)=O FXXACINHVKSMDR-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 230000000397 acetylating effect Effects 0.000 claims abstract description 7
- 230000020477 pH reduction Effects 0.000 claims abstract description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 229960000583 acetic acid Drugs 0.000 claims description 12
- 239000012362 glacial acetic acid Substances 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 9
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 4
- 239000012490 blank solution Substances 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 230000015556 catabolic process Effects 0.000 claims description 3
- 238000006731 degradation reaction Methods 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 230000021736 acetylation Effects 0.000 claims description 2
- 238000006640 acetylation reaction Methods 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 description 5
- -1 aromatic alcohols Chemical class 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 239000011121 hardwood Substances 0.000 description 2
- 239000005457 ice water Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000011122 softwood Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- ANRHNWWPFJCPAZ-UHFFFAOYSA-M thionine Chemical compound [Cl-].C1=CC(N)=CC2=[S+]C3=CC(N)=CC=C3N=C21 ANRHNWWPFJCPAZ-UHFFFAOYSA-M 0.000 description 1
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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
- G01N21/17—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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Abstract
The invention discloses a method for detecting the lignin content of a paper-making pre-cooking liquor, which comprises the following steps: drying lignin in the paper-making pre-cooking liquor, and grinding the lignin into fine powder to obtain a lignin standard sample; taking a proper amount of lignin standard sample, preparing a gradient concentration solution, acetylating lignin by an acidification acetylbromide method, measuring absorbance at 280nm by using an ultraviolet spectrophotometer, and making a standard curve of the absorbance and the lignin concentration; taking a proper amount of the lignin standard sample, detecting the contents of KLASON lignin and acid-soluble lignin by using a KLASON method and an acid-soluble lignin detection method, and correcting the standard curve; and (3) taking a lignin sample to be detected, drying, grinding into fine powder, acetylating lignin, measuring absorbance at 280nm by using an ultraviolet spectrophotometer, and calculating the content of the lignin according to the corrected standard curve. The method for detecting the lignin content of the papermaking pre-cooking liquid has the advantages of high accuracy, good repeatability, short detection time, high efficiency, wide application range and applicability to both high-content and low-content lignin detection.
Description
Technical Field
The invention relates to the field of pulping and papermaking and biomass materials, in particular to a method for detecting the lignin content of a papermaking pre-cooking solution.
Background
Lignin, a class of substances consisting of polymerized aromatic alcohols, is present in woody tissues and primarily functions to harden the cell walls, the major component of secondary walls, by forming a network of cross-links. The lignin is mainly located between the cellulose fibers and plays a role in resisting pressure. Among woody plants, lignin accounts for 25% and is the second most abundant organic matter in the world (cellulose is the first). The lignin is non-toxic, has excellent universality in performance and has wide application in industry. Furthermore, lignin can well replace some non-degradable chemicals and is important for environmental protection.
The lignin has complex components and wide molecular weight distribution, and has no standard substance. The detection of the lignin content has great necessity for the research and application field of the lignin. The most widely used lignin content detection methods are the classical KLASON method and the ultraviolet spectrophotometry method. The KLASON method can accurately detect the content of high-content hardwood lignin, but is not suitable for detecting softwood and herbaceous lignin and low-content hardwood lignin, and has a long detection period. The ordinary ultraviolet spectrophotometry method has the advantages of accurate lignin content, high speed and high repeatability, but the accurate detection can not be realized due to the absence of standard substances. Therefore, the research and development of a new lignin content detection method which is simple, rapid, good in precision and good in repeatability has great significance for the whole papermaking industry.
Disclosure of Invention
The invention aims to provide a method for detecting the lignin content of a paper-making pre-cooking liquor, which aims to overcome the defects in the prior art.
The invention is realized by the following technical scheme:
a method for detecting the lignin content of papermaking pre-cooking liquor comprises the following steps:
drying lignin in a paper-making pre-cooking solution, and grinding the lignin into fine powder to obtain a lignin standard sample;
step two, taking a proper amount of the lignin standard sample, preparing a gradient concentration solution, acetylating the lignin by an acid-catalyzed acetyl bromide method, measuring absorbance at 280nm by an ultraviolet spectrophotometer, and making a standard curve of the absorbance and the lignin concentration;
taking a proper amount of the lignin standard sample, detecting the content of KLASON lignin and acid soluble lignin by using a KLASON method and an acid soluble lignin detection method, and correcting the standard curve;
step four, taking a lignin sample to be detected, drying, grinding into fine powder, acetylating the lignin by an acidification acetyl bromide method, measuring absorbance at 280nm by an ultraviolet spectrophotometer, and calculating the lignin content according to the corrected standard curve:
as a preferred technical scheme, the method for acidifying acetyl bromide is characterized in that the volume ratio of acetyl bromide to glacial acetic acid is 1: 3; the acetylation time is 1.5-2.5 hours, preferably 1 hour and 45 minutes; the temperature of the water bath is 65-75 deg.C, preferably 70 deg.C.
As a preferable technical scheme, before the absorbance is measured, glacial acetic acid is added for dilution, and a proper amount of sodium hydroxide and hydroxylamine hydrochloride are added to eliminate the interference of the background on the absorbance of the lignin. Glacial acetic acid was used as a blank solution in the measurement of absorbance.
As a preferred technical scheme, the method for drying the lignin is drying at 105 ℃ to constant weight.
As a preferred technical scheme, the grinding in the step one and the step four needs to pass through a 100-mesh sieve, so that the dissolution of the solvent is more facilitated.
As a preferred technical scheme, a solution with gradient concentration and lignin to be measured is prepared, and the concentration range is selected to be 0.4-40 mu g/ml, preferably 0.5-35 mu g/ml, and more preferably 0.5-30 mu g/ml.
The KLASON method lignin detection method comprises accurately weighing 1g lignin, adding 20ml 72% sulfuric acid for degradation for 2 hours, transferring into a 1L conical flask, adding 750.64g pure water, continuously adding pure water to keep the liquid level constant, and boiling for 4 hours. Suction filtration is carried out by a weighed G3 sand core crucible, the total volume of filtrate is V (ml), and after taking out and retaining, the solid is washed by water until the solid is neutral. Drying the solid and the crucible at 105 ℃ until the total mass W1 of the solid is measured, and burning the solid and the crucible in a muffle furnace at 575 ℃ until the mass W2 of ash, (W1-W2) x 100 percent, namely the content of KLASON lignin.
The acid soluble lignin content detection method is that the reserved filtrate is diluted by 3 percent sulfuric acid by D times, the 3 percent sulfuric acid is used as a blank to detect the absorbance value A at 205nm, and the acid soluble lignin content is calculated according to the formula:
(W1-W2+ X). times.100% of the total lignin content.
The method for detecting the lignin content of the papermaking pre-cooking liquid has the characteristics that:
1. the curve is corrected by a KLASON and acid-soluble lignin method, so that the accuracy is high and the repeatability is good.
2. The detection time of the lignin content is short, and the detection can be finished by normally detecting for half a day after curve correction.
3. Standard substances are not used, the using amount of the solvent is small, the operation is simple and convenient.
4. A plurality of experiments can be carried out simultaneously, and the efficiency is high.
5. The method has wide application range, and can be used for detecting high-content and low-content lignin.
Detailed Description
The invention is illustrated below by means of specific examples, without being restricted thereto.
Example (b):
1. preparation of lignin samples. 5g of lignin sample of papermaking pre-digestion liquid and 2g of lignin sample to be detected are dried to constant weight at about 105 ℃, ground into fine powder by a mortar, and sieved by a 100-mesh sieve.
2. And (5) drawing a standard curve. Preparing an acidified acetyl bromide solution, acetyl bromide: glacial acetic acid 1:3(V: V). 0.025g of lignin dry powder of the paper-making pre-cooking liquor is taken, and 10ml of acidified acetyl bromide solution is added to prepare 2.5mg/ml storage solution.
A pressure-resistant bottle with a polytetrafluoroethylene sealing cover is used as a digestion hydrolysis bottle, 0.1 ml, 0.2 ml, 0.3 ml, 0.4 ml, 0.5 ml and 0.6ml of storage liquid are respectively taken in the pressure-resistant bottle, 4.9 ml, 4.8 ml, 4.7 ml, 4.6 ml, 4.5ml and 4.4ml of acidified acetyl bromide solution are sequentially added, and each bottle contains 5ml of acidified acetyl bromide with different lignin contents. The temperature of the water bath is kept at 70 ℃ for 1 hour and 45 minutes, and the spinning is performed once every 30 minutes.
Cooling in ice water bath, transferring into 50ml volumetric flask, adding 10ml glacial acetic acid, 4.5ml4N sodium hydroxide and 1.5ml5N hydroxylamine hydrochloride, mixing after adding liquid each time, and finally fixing the volume to 50ml with glacial acetic acid. A series of standard liquors with the same background lignin concentrations of 5, 10, 15, 20, 25, 30. mu.g/ml were formed.
Standing for 30 minutes, taking glacial acetic acid as a blank solution, and detecting an absorbance value at 280nm by using an ultraviolet spectrophotometer 752N (Shanghai cyanine). A linear relationship between absorbance values (a) ═ 0.03 × lignin concentration (μ g/ml) +0.0145, and correlation coefficient ═ 0.9995 was obtained with the solution lignin concentration.
KLASON and acid soluble lignin calibration curves. Accurately weighing 1G of lignin, adding 20ml of 72% sulfuric acid for degradation for 2 hours, transferring the lignin into a 1L conical flask, adding 750.64G of pure water, continuously adding the pure water to keep the liquid level constant, boiling the lignin for 4 hours in an open air, and performing suction filtration by using a weighed G3 sand core crucible. The total volume of the filtrate is 770ml, after taking out and retaining, the solid and the crucible are dried at 105 ℃ until the total mass of the solid W1 is 0.8957g, and the solid and the crucible are burnt in a muffle furnace at 575 ℃ until the mass of ash W2 is 0.0057g, (W1-W2) x 100%, namely the content of KLASON lignin is 89%.
The acid-soluble lignin content detection method is that the reserved filtrate is diluted by 10 times by using 3% sulfuric acid, the 3% sulfuric acid is used as a blank to detect the absorbance value of 0.800A at 205nm, and the acid-soluble lignin content is calculated according to a formula:
(W1-W2+ X). times.100% of the total lignin content is 94.60%.
The corrected curve is: the absorbance value (a) ═ 0.031 × lignin concentration (μ g/ml) +0.0145, and the correlation coefficient ═ 0.9995.
4. Examples of the results of the assay are as follows:
drying lignin to be detected, grinding the lignin into fine powder, weighing 0.0005-0.003g, adding 5ml of acidified acetyl bromide, acetylating the lignin in 70 ℃ water bath for 1 hour and 45 minutes, carrying out ice water bath, transferring the obtained product into a 100ml volumetric flask, adding 10ml of glacial acetic acid, 4.5ml of 4N sodium hydroxide and 1.5ml of hydroxylamine hydrochloride, uniformly mixing after adding liquid for each time, diluting the obtained product to 100ml with glacial acetic acid, measuring absorbance at 280nm by using an ultraviolet spectrophotometer, and calculating the lignin content according to a curve:
TABLE 1 example of test results for lignin samples
| Sample numbering | Mass/g | Concentration of μ g/ml | absorbance/A | Content/% |
| 1 | 0.0015 | 15 | 0.085 | 15.16 |
| 2 | 0.0021 | 21 | 0.265 | 38.48 |
| 3 | 0.0023 | 23 | 0.344 | 46.21 |
| 4 | 0.0027 | 27 | 0.788 | 92.41 |
| 5 | 0.0028 | 28 | 0.678 | 76.44 |
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A method for detecting the lignin content of papermaking pre-cooking liquor is characterized by comprising the following steps:
drying lignin in a paper-making pre-cooking solution, and grinding the lignin into fine powder to obtain a lignin standard sample;
step two, taking a proper amount of the lignin standard sample, preparing a gradient concentration solution, acetylating the lignin by an acid-catalyzed acetyl bromide method, measuring absorbance at 280nm by an ultraviolet spectrophotometer, and making a standard curve of the absorbance and the lignin concentration;
taking a proper amount of the lignin standard sample, detecting the content of KLASON lignin and acid soluble lignin by using a KLASON method and an acid soluble lignin detection method, and correcting the standard curve;
the KLASON method lignin detection method comprises accurately weighing 1g lignin, adding 20ml 72% sulfuric acid for degradation for 2 hours, transferring to a 1L conical flask, adding 750.64g pure water, continuously adding pure water to keep the liquid level constant, and boiling for 4 hours in an open air; carrying out suction filtration by using a weighed G3 sand core crucible, wherein the total volume of filtrate is V, and the unit of the total volume is ml, taking out and reserving the filtrate, and washing the solid to be neutral; drying the solid and the crucible at 105 ℃ until the total mass W1 of the solid is measured by constant weight, and burning the solid and the crucible in a muffle furnace at 575 ℃ until the mass W2 of ash is measured by constant weight, (W1-W2) x 100%, namely the content of KLASON lignin;
in the acid soluble lignin detection method, the reserved filtrate is diluted by 3% sulfuric acid by a factor of D, the 3% sulfuric acid is used as a blank to detect the absorbance value A at 205nm, and the acid soluble lignin content is calculated according to a formula:
(W1-W2+ X) X100% i.e. total lignin content;
step four, taking a lignin sample to be detected, drying, grinding into fine powder, acetylating the lignin by an acidification acetyl bromide method, measuring absorbance at 280nm by an ultraviolet spectrophotometer, and calculating the lignin content according to the corrected standard curve:
the absorbance on the curve corresponds to the concentration in μ g/ml, and the dry weight of the sample corresponds to the concentration in μ g/ml.
2. The method for detecting the lignin content in the paper-making pre-cooking liquor according to claim 1, wherein the acidification of the acetyl bromide method is adopted, wherein the volume ratio of acetyl bromide to glacial acetic acid is 1:3, and the acetylation time is 1.5-2.5 hours; the temperature of the water bath is 65-75 ℃.
3. The method for detecting the lignin content in the paper-making precooking liquor according to claim 2, wherein the acidification of the acetyl bromide method is carried out for 1 hour and 45 minutes; the temperature of the water bath was 70 ℃.
4. The method for detecting the lignin content in the paper-making pre-cooking liquor according to claim 1, wherein before the absorbance is measured, glacial acetic acid is added for dilution, and a proper amount of sodium hydroxide and hydroxylamine hydrochloride are added.
5. The method for detecting the lignin content in the paper-making precooking liquid according to claim 1, characterized in that glacial acetic acid is used as a blank solution in the determination of the absorbance.
6. The method for detecting the lignin content in the paper-making pre-cooking liquor according to claim 1, wherein the lignin is dried at 105 ℃ to constant weight.
7. The method for detecting the lignin content in the paper-making pre-cooking liquor according to claim 1, wherein the grinding in the first step and the fourth step requires a 100-mesh sieve.
8. The method for detecting the lignin content in the paper-making pre-cooking liquor according to claim 1, wherein a solution of lignin to be detected and gradient concentration is prepared, and the concentration range is selected from 0.4 to 40 μ g/ml.
9. The method for detecting the lignin content in the paper-making pre-cooking liquor according to claim 8, wherein a solution of lignin to be detected and gradient concentration is prepared, and the concentration range is selected from 0.5 to 35 μ g/ml.
10. The method for detecting the lignin content in the paper-making pre-cooking liquor according to claim 9, wherein a solution of lignin to be detected and gradient concentration is prepared, and the concentration range is selected from 0.5 to 30 μ g/ml.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01253632A (en) * | 1988-02-26 | 1989-10-09 | Btg Kalle Inventing Ab | Method and apparatus for measuring density of material bonded to particle in fluid medium |
| CN101105444A (en) * | 2007-04-10 | 2008-01-16 | 新疆农业科学院核技术生物技术研究所 | Detection and analysis method for cotton fiber lignin content |
| CN103868778A (en) * | 2014-04-02 | 2014-06-18 | 兰州大学 | Method for measuring lignin content of herbaceous plants |
| CN107228834A (en) * | 2017-07-20 | 2017-10-03 | 山东金科力电源科技有限公司 | Sodium lignosulfonate content test method in premixed compound additive |
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- 2017-10-13 CN CN201710952787.5A patent/CN108872118B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01253632A (en) * | 1988-02-26 | 1989-10-09 | Btg Kalle Inventing Ab | Method and apparatus for measuring density of material bonded to particle in fluid medium |
| CN101105444A (en) * | 2007-04-10 | 2008-01-16 | 新疆农业科学院核技术生物技术研究所 | Detection and analysis method for cotton fiber lignin content |
| CN103868778A (en) * | 2014-04-02 | 2014-06-18 | 兰州大学 | Method for measuring lignin content of herbaceous plants |
| CN107228834A (en) * | 2017-07-20 | 2017-10-03 | 山东金科力电源科技有限公司 | Sodium lignosulfonate content test method in premixed compound additive |
Non-Patent Citations (1)
| Title |
|---|
| Effects of Biomass Accessibility and Klason Lignin Contents during Consolidated Bioprocessing in Populus trichocarpa;Hannah Akinosho et al.;《American Chemical Society》;20170426;第5卷;第5075-5081页 * |
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