CN104655580A - Method for quickly determining content of alpha-cellulose in dissolving pulp - Google Patents
Method for quickly determining content of alpha-cellulose in dissolving pulp Download PDFInfo
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- CN104655580A CN104655580A CN201510072051.XA CN201510072051A CN104655580A CN 104655580 A CN104655580 A CN 104655580A CN 201510072051 A CN201510072051 A CN 201510072051A CN 104655580 A CN104655580 A CN 104655580A
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Abstract
The invention discloses a method for quickly determining the content of alpha-cellulose in dissolving pulp and particularly relates to a method for determining the content of alpha-cellulose in dissolving pulp by virtue of ultraviolet-visible spectrometry. The method comprises the following steps: (1) pre-treating a sample; (2) establishing a standard curve or a mathematical model; (3) detecting the sample by virtue of an ultraviolet/visible spectrophotometer; and (4) calculating to obtain a result. When used for determining the content of alpha-cellulose in dissolving pulp, the method has the beneficial effects that the operation is quick and simple, the detection result can be given within just one hour, and moreover, the result is objective and accurate.
Description
Technical field
The present invention relates to pulping and paper-making and field of textile industry, particularly relate to the method for the alpha-cellulose content in a kind of Fast Measurement dissolving pulp.
Background technology
Dissolving pulp is the high-purity bleached chemical refined stock of a kind of high alpha-cellulose, low hemicellulose and lignin.It is the starting material of multiple chemical products, can prepare multiple cellulose derivative, as made various cellulose ether, cellulose esters etc. by the method for chemistry or physics.Take dissolving pulp as raw material when preparing cellulose derivative product, its purity (being commonly referred to as alpha-cellulose content) has very important impact to the operation of subsequent production cellulose derivative and products thereof quality.Such as, in production process of viscose fiber, the height of its alpha-cellulose content, to the yield of alkali treatment section, the curing carbon amounts consume sulfonation section and obtained viscose rayon quality all play conclusive effect.Therefore, a kind of quick, simple and effective alpha-cellulose content assay method is the important prerequisite implementing dissolving pulp product quality supervision.About the mensuration of alpha-cellulose content in dissolving pulp, traditional method is mainly by the mass ratio of however, residual base cellulose and primary sample after mensuration mercerization, or mensuration alkali cellulose and filtrate are in acid condition by after potassium dichromate oxidation respectively, the ratio of the milliliter number of its l ferrous ammonium sulfate solution consumed separately of titration measuring is adopted to represent the content of alpha-cellulose in slurry.These two kinds of methods are not only consuming time, and complex operation.Therefore, be necessary to develop the content that a kind of new detection method carrys out alpha-cellulose in quick and easy mensuration dissolving pulp.In recent years, someone adopts near-infrared spectrum technique to establish the method directly measuring alpha-cellulose content in plant fiber material in conjunction with chemometrics.But the method does not only have very clear and definite physical significance, and need a large amount of primary samples when modeling and institute's established model has significant limitation.
Shown in (1), alpha-cellulose is the ratio that alkali resistance part accounts for total fibre mass.
W in formula
a,---the quality of alkali resistance cellulose/hemicellulose, g;
W
s---the quality of alkali solubility cellulose/hemicellulose, g;
W
i---the quality of ash content or other impurity, g.
For dissolving pulp, the quality of lignin, ash content or other impurity is negligible.Therefore,
w
α+w
s＝100％ (2)
Therefore, the amount of alpha-cellulose indirectly can be obtained by measuring the alkali-soluble substance be dissolved in filter liquor.As everyone knows, alkali solubility cellulose/hemicellulose can be separated out in ethanol-water solution, generates micron particles, thus makes solution produce turbidity.Therefore, the measuring technology of this analysis of ultraviolet visible spectrometry fast (only needing 1 ~ 2min), (sample is without the need to process) easy and simple to handle, favorable reproducibility can be utilized to measure turbidity, again through mathematical computations, realize measuring the simple fast of alpha-cellulose content in dissolving pulp.So, use the ultraviolet/visible light spectrometry alpha-cellulose content measured in dissolving pulp to be have solid theoretical foundation, and absorption spectrum have significant physical significance.
Summary of the invention
The object of the invention is to the shortcoming and defect overcoming above-mentioned prior art, the method for the alpha-cellulose content in a kind of Fast Measurement dissolving pulp is provided.Overcome the drawback existing for method of alpha-cellulose content in present analysis paper pulp.The present invention adopts alcohol to separate out alkali-soluble substance, makes it produce turbidity in the solution, then adopts ultraviolet/visible color spectrometry to measure the content of alpha-cellulose in dissolving pulp.The method can realize Fast Measurement, and its analysis result accuracy is high, and easy and simple to handle.
The present invention is achieved through the following technical solutions:
A method for alpha-cellulose content in Fast Measurement dissolving pulp, comprises the steps:
(1) sample pretreatment:
Testing sample is put into beaker, in beaker, adds the sodium hydroxide solution that massfraction is 18% or 10%, then beaker is put into water bath with thermostatic control, with tack glass bar compregnate sample repeatedly;
And then add remaining sodium hydroxide solution, and stir;
Finally cover beaker with surface plate, start reaction, and record from first time add NaOH to reaction at the end of time, the time of i.e. mercerization process, after question response terminates, beaker is taken out, and with cleaned and air-dry after glass filter and bottle,suction filter, and collect filtrate with vial with cover; Described testing sample is dissolving pulp;
(2) Criterion curve: by the dissolving pulp of known different alpha-cellulose content after step (1) process, ultraviolet visible spectrometry detection is carried out to gained filtrate, according to the corresponding relation between the alpha-cellulose content in obtained spectral absorbance signal value and known dissolving pulp, obtain a typical curve or a universal model;
(3) sample detection: pipette in filtrate to the 10 ~ 20mL volumetric flask after 0.2-2mL step (1) process with transfer pipet, adding absolute ethyl alcohol is 5 ~ 10mL, finally uses deionized water constant volume, and shakes up mixed liquor; Mixed liquor is poured in cuvette, then carry out ultraviolet visible spectrometry detection, record its spectral absorbance signal value;
(4) result calculates: compared or input universal model by the typical curve of step (3) gained spectral signal value and step (2) gained, obtaining alpha-cellulose content in sample.
Be 2.5 ± 0.05g (claim accurate to 1mg) for pretreated sample absolute dry mass in above-mentioned steps (1), the described compregnate time is 2 ~ 3min, and the time of described mercerization process is 60min, and described water bath with thermostatic control temperature is 20 DEG C ± 2 DEG C; Described beaker volume is 150-mL, and glass filter (model is 1G2) volume is 30-mL, and described bottle,suction volume is 250mL.
When standard model in above-mentioned steps (2) is the dissolving pulp of the different alpha-cellulose content that same raw material prepares, what obtain is typical curve; If step (2) Plays dissolving pulp sample type is unknown, then by multidimensional data disposal methods optic spectrum line, obtain a universal model.
Mensuration wavelength during the described Criterion curve of above-mentioned steps (2) is 500nm; The absorption spectrum characteristic wave bands selected when setting up universal model is 400 ~ 800nm.
When the kind of the slurry sample when testing sample described in above-mentioned steps (4) and Criterion curve is identical, the alpha-cellulose content in sample can be calculated according to the mathematical formulae of typical curve; When testing sample kind is unknown, to original absorbance spectral manipulation, comprises and first order derivative process is carried out to the spectrum of gained, then be input in universal model after smoothing processing is done to curve obtained, experimental results after universal model is analyzed.
Above-mentioned characteristic wave bands extracts the physical significance referred to from absorption spectrum, investigate the factor that absorption spectrum is impacted except alpha-cellulose in dissolving pulp and hemicellulose, if these factors are eliminated by first derivative spectrum process the impact of absorption spectrum, then this factor is ignored, if can not eliminate, then need to reject the wave band that this factor impacts, namely remaining wave band after wave band is rejected in removing is the characteristic wave bands that will extract.
The described method setting up universal model of above-mentioned steps (2) is: the dissolving pulp sample obtaining known alpha-cellulose content from difference slurry factory; Then uv-vis spectra scanning is carried out to the pretreatment filtrates of these samples, the spectrum of acquisition is carried out pre-service, set up the mapping between alpha-cellulose content in feature spectrogram and slurry, thus obtain the universal model of a refining, and this universal model is according to the ultraviolet/visible light spectrum information of input, provides alpha-cellulose content in slurry to be measured.
The present invention, relative to prior art, has following advantage and effect:
The present invention, compared with traditional detection method (GB/T 744-2004), has the following advantages:
First, during the alpha-cellulose content adopting this method to measure in dissolving pulp, do not need the washing (first use pickling, reusable heat distilled water is washed till neutrality) not allowing residue to carry out repeatedly to the alkali obtained after pre-service in step (1);
Secondly, do not need to weigh (generally at least needing 6h) to the alkali undissolved residue constant weight after cleaning yet; Only needing the filtrate to obtaining after pre-service in step (1) to carry out ultraviolet-visible analysis of spectrum (< 10min), then spectroscopic data being brought into the typical curve established in advance or universal model and can obtaining alpha-cellulose content in dissolving pulp.
Therefore, when adopting this method to carry out the alpha-cellulose content in dissolving pulp, not only can simplify the operation flow process, and shorten the test duration (pretreatment time and spectroscopic assay time with about 1h) greatly, testing result can be provided then and there, and result objective and accurate (relative deviation is within 0.5%).Be specially adapted to float rear timely monitoring of starching sample alpha-cellulose content in batch samples analysis and factory floor in laboratory.
Technical measure is easy, is not only suitable for dissolving pulp but also is suitable for lignin and the negligible paper pulp of ash content.
Accompanying drawing explanation
Fig. 1 is the ultraviolet/visible light spectrum absorbance signal value-alkali-soluble substance concentration standard curve in example 1.
Fig. 2 is the first derivative spectrum figure of universal model in example 2.
Fig. 3 is the relation between predicted value and actual value obtained by universal model in example 2.
Embodiment
Below in conjunction with specific embodiment, the present invention is more specifically described in detail.
Embodiment 1
Measure the content of alpha-cellulose in Eucalyptus and Chinese red pine dissolving pulp
(1) sample pretreatment: accurately take the Eucalyptus of the oven dry weight being equivalent to 2.50g (being accurate to 1mg) or Chinese red pine dissolving pulp sample in beaker, the massfraction adding 25mL again in beaker is the sodium hydroxide solution of 18%, again beaker is put into water bath with thermostatic control, with tack glass bar compregnate sample 2 ~ 3min repeatedly.And then add remaining sodium hydroxide solution, and stir it.Finally cover beaker with surface plate.60min consuming time is terminated to reaction adding NaOH from first time.After question response terminates, beaker is taken out, and with cleaned and air-dry after 30-mL 1G2 glass filter and 250-mL bottle,suction filter, and collect filtrate with vial with cover.Described testing sample is dissolving pulp or the negligible paper pulp of lignin content.
(2) Criterion curve: by the Eucalyptus of known different alpha-cellulose content and Chinese red pine dissolving pulp after step (1) process, ultraviolet visible spectrometry detection is carried out to gained filtrate, respective typical curve can be obtained according to the corresponding relation between the alpha-cellulose content in obtained spectral absorbance signal value and dissolving pulp;
(3) sample detection: pipette the filtrate after 1mL step (1) process in 10mL volumetric flask with transfer pipet, add 8mL absolute ethyl alcohol, finally use deionized water constant volume, and shake up mixed liquor.Filtrate is poured in cuvette, then carry out ultraviolet visible spectrometry detection, the spectral absorbance signal value of record sample;
(4) result calculates: compared by the typical curve of step (3) gained spectral signal value and step (2) gained, obtain the content of alpha-cellulose in sample.
(5) measurement result:
Typical curve: C
alpha-cellulose(%)=100-A
q/ k
For masson pine and eucalyptus dissolving pulp, in respective typical curve, k, q value is respectively 0.079,0.5 and 0.092,0.8.
Embodiment 2
Measure the content of the alpha-cellulose in the dissolving pulp of unknown kind
(1) sample pretreatment: accurately take the Eucalyptus of the oven dry weight being equivalent to 2.50g (being accurate to 1mg) or Chinese red pine dissolving pulp sample in beaker, the massfraction adding 25mL again in beaker is the sodium hydroxide solution of 18%, again beaker is put into water bath with thermostatic control, with tack glass bar compregnate sample 2 ~ 3min repeatedly.And then add remaining sodium hydroxide solution, and stir it.Finally cover beaker with surface plate.60min consuming time is terminated to reaction adding NaOH from first time.After question response terminates, beaker is taken out, and with cleaned and air-dry after 30-mL 1G2 glass filter and 250-mL bottle,suction filter, and collect filtrate with vial with cover.Described testing sample is dissolving pulp or the negligible paper pulp of lignin content.
(2) universal model is set up: by the dissolving pulp of the unknown kind of known alpha-cellulose content after step (1) process, ultraviolet visible spectrometry detection is carried out to gained filtrate, first order derivative and smoothing processing are carried out to the ultraviolet-visible spectrogram obtained, recycling chemometrics software set up feature spectrogram and standard dissolution starch in mapping between alpha-cellulose content, thus obtain the universal model of a refining;
(3) sample detection: pipette the filtrate after 1mL step (1) process in 10mL volumetric flask with transfer pipet, add 8mL absolute ethyl alcohol, finally use deionized water constant volume, and shake up mixed liquor.Filtrate is poured in cuvette, then carry out ultraviolet visible spectrometry detection, the spectrogram of record sample;
(4) result exports: be input to by the feature spectrogram that the spectrogram of step (3) gained obtains after first order derivative and smoothing processing in the universal model set up in step (2), automatically the predicted value of an alpha-cellulose is obtained, record numerical value.
(5) measurement result:
Experimental result is shown in accompanying drawing 3.
As mentioned above, just the present invention can be realized preferably.
Embodiment is only for explaining the present invention, and unrestricted the present invention.Other is any do not deviate from Spirit Essence of the present invention and principle under do change, modification, substitute, combine, simplify, all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (7)
1. a method for the alpha-cellulose content in Fast Measurement dissolving pulp, is characterized in that comprising the steps:
(1) sample pretreatment:
Testing sample is put into beaker, in beaker, adds the sodium hydroxide solution that massfraction is 18% or 10%, then beaker is put into water bath with thermostatic control, with tack glass bar compregnate sample repeatedly;
And then add remaining sodium hydroxide solution, and stir;
Finally cover beaker with surface plate, start reaction, and record adds the time at the end of sodium hydroxide solution to reaction from first time, the time of i.e. mercerization process, after question response terminates, beaker is taken out, and with cleaned and air-dry after glass filter and bottle,suction filter, and collect filtrate with vial with cover; Described testing sample is dissolving pulp;
(2) Criterion curve: by the dissolving pulp of known different alpha-cellulose content after step (1) process, ultraviolet visible spectrometry detection is carried out to gained filtrate, according to the corresponding relation between the alpha-cellulose content in obtained spectral absorbance signal value and known dissolving pulp, obtain a typical curve or a universal model;
(3) sample detection: pipette in filtrate to the 10 ~ 20mL volumetric flask after 0.2-2mL step (1) process with transfer pipet, adding absolute ethyl alcohol is 5 ~ 10mL, finally uses deionized water constant volume, and shakes up mixed liquor; Mixed liquor is poured in cuvette, then carry out ultraviolet visible spectrometry detection, record its spectral absorbance signal value;
(4) result calculates: compared or input universal model by the typical curve of step (3) gained spectral signal value and step (2) gained, obtaining alpha-cellulose content in sample.
2. method according to claim 1, it is characterized in that: be 2.5 ± 0.05g (claim accurate to 1mg) for pretreated sample absolute dry mass in step (1), the described compregnate time is 2 ~ 3min, the time of described mercerization process is 60min, and described water bath with thermostatic control temperature is 20 DEG C ± 2 DEG C; Described beaker volume is 150-mL, and glass filter volume is 30-mL, and described bottle,suction volume is 250mL.
3. method according to claim 1 and 2, is characterized in that: when the standard model in step (2) is the dissolving pulp of the different alpha-cellulose content that same raw material prepares, and what obtain is typical curve; If step (2) Plays dissolving pulp sample type is unknown, then by multidimensional data disposal methods optic spectrum line, what obtain is a universal model.
4. method according to claim 1, is characterized in that: mensuration wavelength during the described Criterion curve of step (2) is 500nm; The absorption spectrum characteristic wave bands selected when setting up universal model is 400 ~ 800nm.
5. method according to claim 1, is characterized in that: when the kind of slurry sample when testing sample and Criterion curve is identical, according to the mathematical formulae of typical curve, calculate the alpha-cellulose content in sample;
When testing sample kind is unknown, to original absorbance spectral manipulation, comprises and first order derivative process is carried out to the spectrum of gained, then be input in universal model after smoothing processing is done to curve obtained, experimental results after universal model is analyzed.
6. method according to claim 4, spy is characterised in that: characteristic wave bands extracts the physical significance referred to from absorption spectrum, investigate the factor that absorption spectrum is impacted except alpha-cellulose in dissolving pulp and hemicellulose, if these factors are eliminated by first derivative spectrum process the impact of absorption spectrum, then this factor is ignored, if can not eliminate, then need to reject the wave band that this factor impacts, namely remaining wave band after wave band is rejected in removing is the characteristic wave bands that will extract.
7. method according to claim 5, spy is characterised in that: the foundation of universal model: the dissolving pulp sample obtaining known alpha-cellulose content from difference slurry factory;
Then uv-vis spectra scanning is carried out to the pretreatment filtrates of these samples, the spectrum of acquisition is carried out pre-service, set up the mapping between alpha-cellulose content in feature spectrogram and slurry, thus obtain the universal model of a refining, and this universal model is according to the ultraviolet/visible light spectrum information of input, provides alpha-cellulose content in slurry to be measured.
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| CN104849166A (en) * | 2015-05-26 | 2015-08-19 | 宜宾丝丽雅集团有限公司 | Method for detecting content of alpha cellulose in alkali cellulose |
| CN105300901A (en) * | 2015-10-13 | 2016-02-03 | 华南理工大学 | Method for quickly and accurately determining reactive property of dissolving pulp |
| CN105572260A (en) * | 2016-01-19 | 2016-05-11 | 华南理工大学 | Method for determining alpha-, beta- and gamma- cellulose contents in dissolving pulp |
| CN106979929A (en) * | 2016-01-19 | 2017-07-25 | 中国制浆造纸研究院 | A kind of method of quick measure dissolving pulp reactivity worth |
| CN109738389A (en) * | 2019-01-15 | 2019-05-10 | 西派特（北京）科技有限公司 | Alkali fibre component quantifying test method based on near-infrared spectrum technique |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106979929A (en) * | 2016-01-19 | 2017-07-25 | 中国制浆造纸研究院 | A kind of method of quick measure dissolving pulp reactivity worth |
| CN106979929B (en) * | 2016-01-19 | 2020-05-19 | 中国制浆造纸研究院有限公司 | Method for rapidly determining reaction performance of dissolving pulp |
| CN109738389A (en) * | 2019-01-15 | 2019-05-10 | 西派特（北京）科技有限公司 | Alkali fibre component quantifying test method based on near-infrared spectrum technique |
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