CN107271381B - A kind of method of quick detection nano-cellulose retention in paper - Google Patents
A kind of method of quick detection nano-cellulose retention in paper Download PDFInfo
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- CN107271381B CN107271381B CN201710378549.8A CN201710378549A CN107271381B CN 107271381 B CN107271381 B CN 107271381B CN 201710378549 A CN201710378549 A CN 201710378549A CN 107271381 B CN107271381 B CN 107271381B
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Abstract
The invention discloses a kind of methods of quickly detection nano-cellulose retention in paper, this method is the specific process steps are as follows: carry out dye marker for nano-cellulose first, then the nano-cellulose after dye marker is matched with paper pulp fiber and is copied, with the absorbance of plain boiled water in the molding of spectrophotometry paper, to obtain retention of the nano-cellulose in paper.The present invention can simply and rapidly measure retention of the nano-cellulose in paper by the absorbance of measurement plain boiled water, and the application that the unreasonable loss be capable of timely Instructing manufacture, control nano-cellulose is nano-cellulose in paper industry provides guidance.
Description
Technical field
The invention belongs to pulp and paper technology fields, and in particular to a kind of quickly detection nano-cellulose retention in paper
Method.
Background technique
In recent years, numerous studies report shows that nano-cellulose can effectively improve the physical strength of paper, is expected to conduct
A kind of environmentally protective paper making additive, applies to the enhancing of paper or cardboard.It is timely Instructing manufacture, control in paper production
The unreasonable loss of paper making additive processed, often need to the retention to auxiliary agent measured accurately and in time.Currently, paper making additive stays
The measuring method of rate mainly have calcination method (survey grey point-score), centrifugal separation (measured weight method) and spectrophotometry (colorimetric
Method).In general, calcination method is only applicable to measure retention of the inorganic paper making additive in paper；Centrifugal separation is to pass through
Solid content in measurement plain boiled water is to calculate the retention of paper making additive, but operating process is complicated and accuracy is lower；Light splitting
Photometry is a kind of quick, simple and direct, high-precision detection method, but nano-cellulose is to the no spy of ultraviolet or uv-vis spectra
Levy absorption peak, it is difficult to accurately be detected with this method.Therefore, it is necessary to develop a kind of simpler and more direct, accurate method measurement Nanowire
Retention of the dimension element in paper.
Nano-cellulose dimension fibril belongs to micro-or nano size, and specific surface area with higher has dye molecule extremely strong
Absorption anchoring capability.In addition, dye molecule all has characteristic absorption peak under ultraviolet or uv-vis spectra.Therefore, it uses
Fiber dyes carry out dye marker to nano-cellulose, and there is also identical characteristic absorptions for the nano-cellulose after dye marker
Peak.In paper-making process, the absorbance of the nano-cellulose of dye marker in plain boiled water is measured, will simple and direct, accurately be detected
Its retention in paper.
Summary of the invention
The purpose of the invention is to overcome the shortcomings of existing measurement paper making additive retention method in paper, will first receive
Rice cellulose carries out dye marker, then is matched with the nano-cellulose after dye marker with paper pulp fiber and copied.By in measurement plain boiled water
The absorbance of nanofiber fibril, to realize simple and direct, accurately retention of the measurement nanofiber fibril in paper-making process.
The purpose of the present invention is achieved through the following technical solutions.
A kind of method of quick detection nano-cellulose retention in paper, method includes the following steps:
By lignocellulosic slurry carry out enzymolysis processing after, then ground, dye marker, it is high-pressure homogeneous processing contaminated
It is measured the absorbance of plain boiled water with copying with paper pulp fiber by the nano-cellulose for expecting label.
Preferably, this method specifically includes the following steps:
(1) lignocellulosic slurry is subjected to defibrination process；
(2) step (1) treated slurry is subjected to enzymolysis processing；
(3) slurry after step (2) enzymatic treatment is subjected to nanosizing mechanical lapping processing；
(4) dye marker is carried out to slurry after step (3) nanosizing mechanical lapping processing；
(5) slurry after step (4) dye marker is continued into high-pressure homogeneous processing；
(6) match with paper pulp with the nano-cellulose after step (5) homogeneous and copy, and it is after molding white to collect paper
Water；
(7) with the absorbance of plain boiled water obtained by spectrophotometry determination step (6).
It is further preferred that the concentration of slurry is 10 wt%-30 wt% after defibrination process in step (1).
It is further preferred that in step (2), slurry concentration is 1 wt%-10 wt%, pH 4.5- when the enzymolysis processing
6, temperature is 35-60 DEG C, time 5-40h.
It is further preferred that the enzyme is the enzyme that fibre structure can be made loose in step (2).
It is further preferred that the enzyme is cellulose complex enzyme, mashing enzyme or restriction endonuclease.
It is further preferred that slurry concentration is 0.1 wt ‰ -1.5 when the mechanical lapping is handled in step (3)
Wt ‰, pressure are 0-60 MPa.
It is further preferred that in step (4), the temperature that when dyeing stirs is 30-90 DEG C, and revolving speed is 50-800 r/
Min, time are 5-36 h.
It is further preferred that the dosage of the dyestuff is 50g/kg -200g/kg oven dry stock in step (4).
It is further preferred that homogeneous internal fluid pressure is 70-250 in the high-pressure homogeneous processing in step (5)
MPa。
It is further preferred that carrying out constant volume to the plain boiled water of collection in step (6).
It is further preferred that the absorbing wavelength of spectrophotometer is 200-800 nm in step (7).
It is further preferred that specific step is as follows for this method:
(1) cellulose paste is subjected to defibrination process, slurry concentration is between 10%-25%；
(2) treated slurry is digested, slurry concentration 1%-10%, pH 4.5-6, temperature 40-60
DEG C, enzymolysis time 5-36h；
(3) slurry after above-mentioned enzymatic hydrolysis is subjected to nanosizing mechanical lapping processing, it is 0.01%-1.5%, pressure that it is dense, which to adjust slurry,
For 0-400MPa；
(4) a certain amount of dye solution is added in the slurry after the mechanical lapping of Xiang Shangshu nanosizing, and stirs, revolving speed 500-
800 r/min, temperature are 50-80 DEG C；
(5) slurry after above-mentioned dye marker is subjected to high-pressure homogeneous processing, homogenization pressure 70-250MPa；
(6) nano-cellulose after above-mentioned homogeneous collect paper plain boiled water after molding with copying and detect with paper pulp
Its absorbance.
Compared with prior art, the present invention have it is following the utility model has the advantages that
(1) nano-cellulose of the dye marker obtained by the present invention does not fade in water, can accurately reflect Nanowire
Content of the dimension element in plain boiled water；
(2) present invention can simple and direct, rapidly measure retention of the nano-cellulose in paper pulp, can instruct to give birth in time
It produces, the unreasonable loss of control nano-cellulose.
Detailed description of the invention
Fig. 1 is the absorbance figure of nano-cellulose after dye marker under different incident wavelengths.
Fig. 2 is absorbance curve figure of the nano-cellulose under 504 nm wavelength after dye marker.
Specific embodiment
Specific implementation of the invention is described in further detail below in conjunction with example, but embodiments of the present invention are not
It is limited to this.
The present invention is not particularly limited the type of lignocellulosic material used, source, below with direct scarlet
For dyestuff and softwood pulp.
Embodiment 1
(1) 60g needlebush slurry is subjected to defibrination process, slurry concentration is 10 wt% after processing；
(2) by step (1), treated, and slurry is digested, first cellulose complex enzyme (enzyme activity is 180 PFU/g)
It is dissolved in deionized water, obtains cellulase solution；Adjusting slurry concentration with enzymolysis liquid again is 5 wt%, and enzyme dosage is 50g/kg(phase
For oven dry stock), 3 h of enzymatic treatment at being 5.5,50 DEG C in pH；
(3) slurry after step (2) enzymatic treatment is subjected to mechanical lapping processing, when mechanical lapping adds deionized water to adjust slurry
Material concentration is 1 wt ‰, is ground 4 times under 40MPa pressure；
(4) it will be added in direct scarlet 4B after the slurries filtration after step (3) grinding, wherein the dosage of direct scarlet 4B
For 100g/kg (relative to oven dry stock), stirring 4h is dyed under the conditions of being 300 r/min in 50 DEG C, revolving speed；
(5) it will be put into after slurries filtration obtained by step (4) and carry out high pressure in super-pressure nanometer homogenizer (Nano DeBEE)
Homogenization, homogenization pressure 100MPa obtain the nano-cellulose of dye marker；
(6) matched with the nano-cellulose of the homogeneous rear dye marker of step (5) with softwood pulp and copied, the Nanowire of dye marker
The additive amount of dimension element is 1 wt% (relative to oven dry stock), collects paper plain boiled water after molding and is settled to 500 ml；
(7) under 504nm wavelength plain boiled water collected by detecting step (6) absorbance.
As a result: the nano-cellulose of gained dye marker has characteristic absorption peak at wavelength 504nm, as shown in Figure 1.It will dye
The nano-cellulose of material label is configured to various concentration (100mg/ml, 200 mg/ml, 400 mg/ml, 600 mg/ml, 800
Mg/ml, 1000mg/ml), the relationship between absorbance and concentration is that Y=0.0015X(is as shown in Figure 2).The suction of gained plain boiled water
Luminosity is 0.043, and nanofiber cellulose content is 14.22 mg in plain boiled water, and the content of nano-cellulose is 4.6mg, nanometer in paper
Retention of the cellulose in paper is 24.54%, and detection time is 5 min.
After carrying out centrifugal drying to the solid content in plain boiled water using weight method, received in paper obtained by weighing detecting step (6)
The retention of rice cellulose is 24.63%, and detection time is 24 h.
Embodiment 2
(1) 60g needlebush slurry is subjected to defibrination process, slurry concentration is 15wt% after processing；
(2) by step (1), treated, and slurry is digested, first cellulose complex enzyme (enzyme activity is 180 PFU/g)
It is dissolved in deionized water, obtains cellulase solution；Adjusting slurry concentration with enzymolysis liquid again is 2wt%, and enzyme dosage is 50g/kg(phase
For oven dry stock), it is 5.5 in pH, 36 h of enzymatic treatment at 40 DEG C；
(3) slurry after step (2) enzymatic treatment is subjected to mechanical lapping processing, when mechanical lapping adds deionized water to adjust slurry
Material concentration is 1 wt ‰, is ground 4 times in the case where pressure is 60MPa；
(4) it will be added in direct scarlet 4B after the slurries filtration after step (3) grinding, wherein the dosage of direct scarlet 4B is
100g/kg (relative to oven dry stock) stirs 7 h under the conditions of being 900r/min in 60 DEG C, revolving speed and is dyed；
(5) it will be put into after slurries filtration obtained by step (4) and carry out high pressure in super-pressure nanometer homogenizer (Nano DeBEE)
Homogenization, homogenization pressure 200MPa obtain the nano-cellulose of dye marker；
(6) matched with the nano-cellulose of the homogeneous rear dye marker of step (5) with softwood pulp and copied, the Nanowire of dye marker
The additive amount of dimension element is 12wt% (relative to oven dry stock), collects paper plain boiled water after molding and is settled to 500 ml；
(7) under 504nm wavelength plain boiled water collected by detecting step (6) absorbance.
As a result: according to the relationship (as shown in Figure 2) between absorbance and the nano-cellulose concentration of dye marker, gained is white
The absorbance of water is 0.406, and nanofiber cellulose content is 135.27mg in plain boiled water, and the content of nano-cellulose is in paper
90.8mg, retention of the nano-cellulose in paper are 40.17%, and detection time is 5 min.
After carrying out centrifugal drying to the solid content in plain boiled water using weight method, received in paper obtained by weighing detecting step (6)
The retention of rice cellulose is 40.31%, and detection time is 24 h.
Embodiment 3
(1) 60g needlebush slurry is subjected to defibrination process, slurry concentration is 25wt% after processing；
(2) by step (1), treated, and slurry is digested, first cellulose complex enzyme (enzyme activity is 180 PFU/g)
It is dissolved in deionized water, obtains cellulase solution；Adjusting slurry concentration with enzymolysis liquid again is 10wt%, and enzyme dosage is 50g/kg(phase
For oven dry stock), it is 4.8 in pH, 15 h of enzymatic treatment at 60 DEG C；
(3) slurry after step (2) enzymatic treatment is subjected to mechanical lapping processing, when mechanical lapping adds deionized water to adjust slurry
Material concentration is 1 wt ‰, is ground 4 times in the case where pressure is 40MPa；
(4) it will be added in direct scarlet 4B after the slurries filtration after step (3) grinding, wherein the dosage of direct scarlet 4B is
100g/kg (relative to oven dry stock), stirring 12h is dyed under the conditions of being 200r/min in 70 DEG C, revolving speed；
(5) it will be put into after slurries filtration obtained by step (4) and carry out high pressure in super-pressure nanometer homogenizer (Nano DeBEE)
Homogenization, homogenization pressure 250MPa obtain the nano-cellulose of dye marker；
(6) nano-cellulose of the dye marker with step (5) after homogeneous is matched with softwood pulp and is copied, the nanometer of dye marker
The additive amount of cellulose is 30wt% (relative to oven dry stock), collects paper plain boiled water after molding and is settled to 500 ml；
(7) under 504nm wavelength plain boiled water collected by detecting step (6) absorbance.
As a result: according to the relationship (as shown in Figure 2) between absorbance and the nanofiber concentration of dye marker, gained plain boiled water
Absorbance be 0.798, nanofiber cellulose content is 265.93mg in plain boiled water, and the content of nano-cellulose is in paper
299.3mg, retention of the nano-cellulose in paper are 52.95%, and detection time is 5 min.
After carrying out centrifugal drying to the solid content in plain boiled water using weight method, received in paper obtained by weighing detecting step (6)
The retention of rice cellulose is 54.85 %, and detection time is 24 h.
The nano-cellulose of the resulting dye marker of the present invention described above can it is simple and direct, rapidly measure nano-cellulose
Retention in paper pulp, timely Instructing manufacture, the unreasonable loss for controlling nano-cellulose.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by the embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications done without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (9)
1. a kind of method of quickly detection nano-cellulose retention in paper, which is characterized in that this method includes following step
It is rapid:
(1) lignocellulosic slurry is subjected to defibrination process；
(2) slurry after step (1) defibrination process is subjected to enzymolysis processing；The enzyme of the enzymatic hydrolysis is that fibre structure can be made loose
Enzyme；
(3) slurry after step (2) enzymatic hydrolysis is subjected to mechanical lapping processing；
(4) dye marker will be carried out after slurries filtration obtained by step (3)；
(5) slurry after step (4) dye marker is subjected to high-pressure homogeneous processing；
(6) nano-cellulose after the dye marker obtained by step (5) is matched with paper pulp fiber copies, and it is after molding white to collect paper
Water；
(7) absorbance of plain boiled water obtained by spectrophotometer determination step (6).
2. a kind of method of quickly detection nano-cellulose retention in paper according to claim 1, feature exist
In: in step (1), the concentration of slurry is 10 wt%-30 wt% after defibrination process.
3. a kind of method of quickly detection nano-cellulose retention in paper according to claim 1, feature exist
In: in step (2), slurry concentration is 1 wt%-10 wt% when the enzymolysis processing.
4. a kind of method of quickly detection nano-cellulose retention in paper according to claim 1, feature exist
In: in step (2), the pH when enzymolysis processing is 4.5-6, and temperature is 35-60 DEG C, time 2-40h.
5. a kind of method of quickly detection nano-cellulose retention in paper according to claim 1, feature exist
In: the enzyme of the enzymatic hydrolysis is cellulose complex enzyme, mashing enzyme or restriction endonuclease.
6. a kind of method of quickly detection nano-cellulose retention in paper according to claim 1, feature exist
In: in step (3), slurry concentration is 0.1 wt, ‰ -3 wt ‰ when the mechanical lapping is handled, and pressure is 0-60 MPa.
7. a kind of method of quickly detection nano-cellulose retention in paper according to claim 1, feature exist
In: in step (4), temperature is 30-90 DEG C when the dye marker, and revolving speed is 50-1000 r/min, and the time is 1-48 h.
8. a kind of method of quickly detection nano-cellulose retention in paper according to claim 1, feature exist
In: in step (4), the dosage of the dyestuff is 50g/kg-200g/kg oven dry stock.
9. a kind of method of quickly detection nano-cellulose retention in paper according to claim 1, feature exist
In: in step (5), homogenizer internal fluid pressure is 60-250MPa in the high-pressure homogeneous processing.
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| CN107894500A (en) * | 2017-10-26 | 2018-04-10 | 华南理工大学 | A kind of method of quantitative measurment plant micro-nano cellulose retention in paper making process |
| CN108007905A (en) * | 2017-10-26 | 2018-05-08 | 华南理工大学 | A kind of method of quantitatively characterizing micro-nano cellulose turnover rate in paper making process |
| CN108517712A (en) * | 2018-03-12 | 2018-09-11 | 华南理工大学 | A kind of paper grade (stock) micro nanometer fiber mill base and the preparation method and application thereof |
| CN108497543B (en) * | 2018-03-30 | 2021-05-14 | 昆明理工大学 | Method for evaluating retention effect of retention aid on paper-making reconstituted tobacco slurry |
| CN110106736A (en) * | 2019-04-18 | 2019-08-09 | 华南理工大学 | A kind of environmental type anti-counterfeiting paper and preparation method thereof |
| CN110080028B (en) * | 2019-04-18 | 2021-06-08 | 华南理工大学 | Method for improving color fastness of paper or paperboard |
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