CN108872118A - A kind of detection method of papermaking pre-cooked liquid content of lignin - Google Patents
A kind of detection method of papermaking pre-cooked liquid content of lignin Download PDFInfo
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- CN108872118A CN108872118A CN201710952787.5A CN201710952787A CN108872118A CN 108872118 A CN108872118 A CN 108872118A CN 201710952787 A CN201710952787 A CN 201710952787A CN 108872118 A CN108872118 A CN 108872118A
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- 229920005610 lignin Polymers 0.000 title claims abstract description 102
- 238000001514 detection method Methods 0.000 title claims abstract description 38
- 239000007788 liquid Substances 0.000 title claims abstract description 29
- 238000002835 absorbance Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 19
- FXXACINHVKSMDR-UHFFFAOYSA-N acetyl bromide Chemical compound CC(Br)=O FXXACINHVKSMDR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 12
- 230000021736 acetylation Effects 0.000 claims abstract description 11
- 238000006640 acetylation reaction Methods 0.000 claims abstract description 11
- 230000020477 pH reduction Effects 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 16
- 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
- 238000001035 drying Methods 0.000 claims description 9
- 239000012362 glacial acetic acid Substances 0.000 claims description 9
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000002023 wood Substances 0.000 claims description 5
- 239000012490 blank solution Substances 0.000 claims description 3
- 150000001262 acyl bromides Chemical class 0.000 claims 2
- 230000008033 biological extinction Effects 0.000 claims 1
- 238000010790 dilution Methods 0.000 claims 1
- 239000012895 dilution Substances 0.000 claims 1
- 238000005259 measurement Methods 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 12
- 239000007787 solid Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000011121 hardwood Substances 0.000 description 2
- 239000005457 ice water Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000007799 cork Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000029087 digestion Effects 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
- 239000000203 mixture Substances 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
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000005406 washing Methods 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
- G01N21/17—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)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a kind of detection methods of papermaking pre-cooked liquid content of lignin, include the following steps：Papermaking pre-cooked liquid lignin is dried, fine powder is ground into, obtains lignin standard specimen；Appropriate lignin standard specimen is taken, gradient concentration solution is prepared, using acidification acetyl bromide method acetylation lignin, absorbance is measured at 280nm with ultraviolet specrophotometer, makes the standard curve of absorbance and lignin concentration；The appropriate lignin standard specimen is taken, with KLASON method and the molten lignin detection method detection KLASON lignin of acid and the molten content of lignin of acid, corrects the standard curve；Lignin sample to be measured is taken, dries, is ground into fine powder, acetylation lignin measures absorbance with ultraviolet specrophotometer at 280nm, calculates content of lignin according to the standard curve after the correction.Papermaking pre-cooked liquid content of lignin is detected using the present invention, accuracy rate is higher, and reproducible, detection time is short, and high-efficient, applied widely, high-content, the detection of low content lignin are applicable.
Description
Technical field
The present invention relates to pulping and paper-making and biological material fields, and in particular to a kind of papermaking pre-cooked liquid content of lignin
Detection method.
Background technique
Lignin is the substance being made of the aromatic alcohol polymerizeing, and is present in lignum, and main function is to pass through
It forms intertexture net and carrys out sclereid wall, be secondary wall main component.Lignin is predominantly located between cellulose fibre, is played resistance to compression and is made
With.In xylophyta, lignin accounts for 25%, is the most abundant organic matter of second in the world (cellulose is first).Wood
Quality is nontoxic, has fabulous versatility in aspect of performance, is industrially widely used.Moreover, lignin can replace well
It is critically important for our environmental protection for some nondegradable chemicals.
Lignin component is complicated, and molecular weight distribution is wide, without standard substance.The detection of content of lignin, to lignin
Research application field has very big necessity.It the use of most wide content of lignin detection method is classical KLASON method, ultraviolet
Spectrophotometry.Although KLASON method can accurately detect the content of high-content hardwood lignin, be not suitable for cork and grass
The detection of this lignin and low content hardwood lignin, and detection cycle is longer.General ultraviolet spectrophotometry just detects wood
Lignin content is accurate, speed is fast, repeatability is high, but due to not having standard substance that can not accomplish accurately to detect.So researching and developing one kind
It is new it is simple rapidly, precision is good and reproducible content of lignin detection method for entire paper industry with very big
Meaning.
Summary of the invention
The object of the present invention is to provide a kind of detection methods of papermaking pre-cooked liquid content of lignin, to solve background technique
Existing drawbacks described above.
Of the invention realizes by the following technical solutions：
A kind of detection method of papermaking pre-cooked liquid content of lignin, includes the following steps：
Papermaking pre-cooked liquid lignin is dried, is ground into fine powder, obtains lignin standard specimen by step 1；
Step 2 takes the appropriate lignin standard specimen, prepares gradient concentration solution, then using acidification acetyl bromide method acetyl
Change lignin, measure absorbance at 280nm with ultraviolet specrophotometer, the standard for making absorbance and lignin concentration is bent
Line；
Step 3 takes the appropriate lignin standard specimen, with KLASON method and the molten lignin detection method detection KLASON wood of acid
Quality and the molten content of lignin of acid, correct the standard curve；
Step 4 takes lignin sample to be measured, drying, be ground into fine powder, using acidification acetyl bromide method acetylation lignin,
Absorbance is measured at 280nm with ultraviolet specrophotometer, and content of lignin is calculated according to the standard curve after the correction：
The acidification acetyl bromide method as a preferred technical solution, wherein the volume ratio of acetyl bromide and glacial acetic acid is 1:3；
The acetylation time is 1.5-2.5 hours, preferably 45 minutes 1 hour；Bath temperature is 65-75 DEG C, preferably 70 DEG C.
The acetylation lignin also needs ice acetic acid to dilute before measuring absorbance as a preferred technical solution, and
Appropriate sodium hydroxide and hydroxylamine hydrochloride is added, to eliminate interference of the background to lignin absorbance.When measuring absorbance, with ice
Acetic acid makees blank solution.
The method for drying lignin as a preferred technical solution, is 105 DEG C, and drying to constant weight.
It is ground described in step 1 and step 4 as a preferred technical solution, is to need to sieve with 100 mesh sieve, it is more conducively molten
The dissolution of agent.
The solution of gradient concentration and lignin to be measured is prepared as a preferred technical solution, and the range selection of concentration exists
0.4-40 μ g/ml, preferably 0.5-35 μ g/ml, more preferably 0.5-30 μ g/ml.
KLASON method lignin detection method is accurate weighing 1g lignin, and 20ml72% sulfuric acid is added and degrades 2 hours, turns
It moves on in 1L conical flask, 750.64g pure water is added, constantly plus pure water keeps liquid level constant, and opening is boiled 4 hours.With weighed
G3 sand core crucible filter, filtrate total volume is V (ml), is taken out after retaining, and washing solid is to neutrality.Solid and 105 DEG C of crucible
Drying to constant weight measures solid gross mass W1, solid and crucible and burns in 575 DEG C of Muffle furnaces to constant weight and measure ash content quality W2,
It (W1-W2) × 100% is KLASON content of lignin.
The molten content of lignin detection method of acid is that the filtrate retained dilutes D times with 3% sulfuric acid, is sky with 3% sulfuric acid
Absorbance value A at white detection 205nm calculates the molten content of lignin of acid according to formula：
It (W1-W2+X) × 100% is total lignin levels.
It is using the characteristics of present invention detection papermaking pre-cooked liquid content of lignin：
1. curve is by KLASON and the molten lignin method correction of acid, accuracy rate is higher, reproducible.
2. content of lignin detection time is short, normally detects to can be detected half a day after curvature correction and finish.
3. not using standard substance, solvent usage amount is few, convenient, easy to operate.
4. multiple experiments can be carried out simultaneously, it is high-efficient.
5. applied widely, high-content, the detection of low content lignin are applicable.
Specific embodiment
The present invention is illustrated below by specific embodiment, but is not intended to limit the present invention.
Embodiment：
1. the preparation of lignin sample.Papermaking pre-cooked liquid lignin sample 5g and lignin sample 2g to be measured or so 105
DEG C drying to constant weight, with mortar grinder at fine-powdered, sieves with 100 mesh sieve.
2. the drafting of standard curve.Prepare acidification acetyl bromide solution, acetyl bromide：Glacial acetic acid=1:3(V:V).Take papermaking pre-
Cooking liquor lignin dry powder 0.025g is added 10ml and is acidified acetyl bromine solutions, is configured to the storing liquid of 2.5mg/ml.
Use the pressure bottle that covers with polytetrafluoroethylene (PTFE) to hydrolyze bottle as digestion, take 0.1 respectively, 0.2,0.3,0.4,0.5,
0.6ml storing liquid sequentially adds 4.9,4.8,4.7,4.6,4.5,4.4ml acidification acetyl bromine solutions, makes every bottle in pressure bottle
In the equal acidification acetyl bromides containing 5ml, and content of lignin is different.70 DEG C of water-baths keep the temperature 45 minutes 1 hour, light every 30 minutes
Rotation is primary.
Ice-water bath is cooling, is transferred in 50ml volumetric flask, and 10ml glacial acetic acid, 4.5ml4N sodium hydroxide and 1.5ml5N is added
Hydroxylamine hydrochloride mixes after each liquid feeding, finally with glacial acetic acid constant volume to 50ml.Forming the lignin concentration with same background is
5, the series standard liquid of 10,15,20,25,30 μ g/ml.
30 minutes are stood, using glacial acetic acid as blank solution, with ultraviolet specrophotometer 752N (Shanghai essence) at 280nm
Detect absorbance value.Obtain the linear relationship between absorbance value and solution lignin concentration, absorbance value (A)=0.03 × wood
Quality concentration (μ g/ml)+0.0145, related coefficient=0.9995.
3.KLASON and the molten lignin calibration curve of acid.It is small that the degradation 2 of 20ml72% sulfuric acid is added in accurate weighing 1g lignin
When, it is transferred in 1L conical flask, 750.64g pure water is added, constantly plus pure water keeps liquid level constant, and opening is boiled 4 hours, with title
The G3 sand core crucible crossed again filters.Filtrate total volume is V=770ml, is taken out after retaining, and solid and 105 DEG C of crucible are dried to perseverance
It resurveys out solid gross mass W1=0.8957g, solid and crucible and burns in 575 DEG C of Muffle furnaces to constant weight and measure ash content quality W2=
0.0057g, (W1-W2) × 100% are KLASON content of lignin 89%.
The molten content of lignin detection method of acid is that the filtrate retained dilutes 10 times with 3% sulfuric acid, is sky with 3% sulfuric acid
Absorbance value 0.800A at white detection 205nm calculates the molten content of lignin of acid according to formula：
It (W1-W2+X) × 100% is total lignin levels 94.60%.
Curve after correction is：Absorbance value (A)=0.031 × lignin concentration (μ g/ml)+0.0145, related coefficient
=0.9995.
4. detection fructufy for example under：
The lignin drying for taking needs to detect, is ground into fine powder, weighs 0.0005-0.003g, 5ml is added to be acidified acetyl bromide 70
DEG C water-bath acetylation lignin 45 minutes 1 hour, ice-water bath was transferred in 100ml volumetric flask, be added 10ml glacial acetic acid,
4.5ml4N sodium hydroxide, 1.5ml hydroxylamine hydrochloride mix after each liquid feeding, with glacial acetic acid constant volume to 100ml, with ultraviolet spectrometry light
Degree meter measures absorbance at 280nm, calculates content of lignin according to curve：
1. lignin sample detection result example of table
| Sample number into spectrum | Quality/g | Concentration 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 above shows and describes the basic principle, main features and advantages of the invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (10)
1. a kind of detection method of papermaking pre-cooked liquid content of lignin, which is characterized in that include the following steps：
Papermaking pre-cooked liquid lignin is dried, is ground into fine powder, obtains lignin standard specimen by step 1；
Step 2 takes the appropriate lignin standard specimen, prepares gradient concentration solution, then using acidification acetyl bromide method acetylation wood
Quality measures absorbance with ultraviolet specrophotometer at 280nm, makes the standard curve of absorbance and lignin concentration；
Step 3 takes the appropriate lignin standard specimen, detects KLASON lignin with KLASON method and the molten lignin detection method of acid
With the molten content of lignin of acid, the standard curve is corrected；
Step 4 takes lignin sample to be measured, and drying is ground into fine powder, using acidification acetyl bromide method acetylation lignin, with purple
Outer spectrophotometer measures absorbance at 280nm, calculates content of lignin according to the standard curve after the correction：
2. the detection method of papermaking pre-cooked liquid content of lignin as described in claim 1, which is characterized in that the acidification second
Acylbromide method, wherein the volume ratio of acetyl bromide and glacial acetic acid is 1:3, the acetylation time is 1.5-2.5 hours；Bath temperature is 65-
75℃。
3. the detection method of papermaking pre-cooked liquid content of lignin as claimed in claim 2, which is characterized in that the acidification second
Acylbromide method, wherein the acetylation time is 45 minutes 1 hour；Bath temperature is 70 DEG C.
4. the detection method of papermaking pre-cooked liquid content of lignin as described in claim 1, which is characterized in that the acetylation
Lignin is before measuring absorbance, ice acetic acid dilution, and appropriate sodium hydroxide and hydroxylamine hydrochloride is added.
5. the detection method of papermaking pre-cooked liquid content of lignin as described in claim 1, which is characterized in that in measurement extinction
When spending, blank solution is made with glacial acetic acid.
6. the detection method of papermaking pre-cooked liquid content of lignin as described in claim 1, which is characterized in that drying lignin
Method be 105 DEG C drying to constant weight.
7. the detection method of papermaking pre-cooked liquid content of lignin as described in claim 1, which is characterized in that step 1 and step
It is ground described in rapid four, needs to sieve with 100 mesh sieve.
8. the detection method of papermaking pre-cooked liquid content of lignin as described in claim 1, which is characterized in that it is dense to prepare gradient
The range of the solution of degree and lignin to be measured, concentration is selected in 0.4-40 μ g/ml.
9. the detection method of papermaking pre-cooked liquid content of lignin as claimed in claim 8, which is characterized in that it is dense to prepare gradient
The range of the solution of degree and lignin to be measured, concentration is selected in 0.5-35 μ g/ml.
10. the detection method of papermaking pre-cooked liquid content of lignin as claimed in claim 9, which is characterized in that prepare gradient
The range of the solution of concentration and lignin to be measured, concentration is selected in 0.5-30 μ g/ml.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2784776C1 (en) * | 2022-07-12 | 2022-11-29 | Федеральное государственное бюджетное учреждение науки Федеральный исследовательский центр "КОМИ научный центр Уральского отделения Российской академии наук" | Method for determining the mass concentration of lignin substances in natural, waste and treated waste water |
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
- 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 (3)
| Title |
|---|
| HANNAH AKINOSHO ET AL.: "Effects of Biomass Accessibility and Klason Lignin Contents during Consolidated Bioprocessing in Populus trichocarpa", 《AMERICAN CHEMICAL SOCIETY》 * |
| 王建庆等: "乙酰溴法测定棉籽壳中木质素的含量", 《纺织学报》 * |
| 胡磊: "《环境生态监测实验教程》", 30 June 2017 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2784776C1 (en) * | 2022-07-12 | 2022-11-29 | Федеральное государственное бюджетное учреждение науки Федеральный исследовательский центр "КОМИ научный центр Уральского отделения Российской академии наук" | Method for determining the mass concentration of lignin substances in natural, waste and treated waste water |
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Effective date of registration: 20210802 Address after: Room 322, building 32, 680 Guiping Road, Xuhui District, Shanghai, 200233 Patentee after: SHANGHAI CHANGFA NEW MATERIAL Co.,Ltd. Address before: 272101 Industrial Park, Xinglongzhuang Town, Yanzhou District, Jining City, Shandong Province Patentee before: JINING MINGSHENG NEW MATERIAL Co.,Ltd. |