CN106124267B - A kind of method of quantitative measurment bacteria cellulose retention in paper making process - Google Patents
A kind of method of quantitative measurment bacteria cellulose retention in paper making process Download PDFInfo
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- CN106124267B CN106124267B CN201610515263.5A CN201610515263A CN106124267B CN 106124267 B CN106124267 B CN 106124267B CN 201610515263 A CN201610515263 A CN 201610515263A CN 106124267 B CN106124267 B CN 106124267B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/227—Measuring photoelectric effect, e.g. photoelectron emission microscopy [PEEM]
Abstract
The invention discloses a kind of methods of quantitative measurment bacteria cellulose retention in paper making process.Bacteria cellulose of the present invention is to secrete the cellulose synthesized by bacterial micro-organism at different conditions.The microorganism of eccrine fiber element includes acetic acid Pseudomonas, Agrobacterium, pseudomonas, achromobacter, alcaligenes, Aerobacter, azotobacter, rhizobium and Sarcina etc..Paper making additive refers to the additive that can improve physical properties of paper added in lumber fibre, non-wood plant fibre or secondary stock slurry paper making process.The method of quantitative measurment bacteria cellulose retention in paper-making process of the present invention, it is the group for having nitrogen in grafting on the hydroxyl of bacteria cellulose molecule, nitrogen element content in paper is measured by elemental analyser or x-ray photoelectron spectroscopy, the retention of bacteria cellulose is calculated with this.Quantitative detecting method of the invention can achieve the Accurate Determining to retention.
Description
Technical field
The present invention relates to the fields of measurement of retention, and in particular to a kind of quantitative measurment bacteria cellulose is in paper making mistake
The method of retention in journey.
Background technique
Secondary stock and non-wood fibrous raw material occupy very big specific gravity in China's paper industry.However, most of
Secondary stock and non-wood-fiber base paper physical property are slightly lower, do not adapt to modern industry to high-performance paper based composites
Demand, thus research and develop efficient paper strengthening agent and be of great significance;Demand of the China to functional paper-based article is also more next simultaneously
It is bigger.
Bacteria cellulose is a kind of emerging biomaterial, is synthesized by microorganism secretion, has high cellulose purity
And crystallinity, fine microcosmic reticular structure, the physical strength of paper can be effectively improved by being combined into paper with plant fiber.In addition,
By means of bacteria cellulose and plant fiber, binding ability by the chemical modification to bacteria cellulose promotes its function strongly
Characteristic can be changed, and assign paper specific function, it may have ideal effect.
For the combination effect for improving bacteria cellulose and plant fiber, the bacteria cellulose size after mechanical dispersion is general
It is smaller, it is most likely that as moisture flows away in paper-making process, thus to study retention and preparation bacteria cellulose-base papermaking is helped
Agent is of great significance.However since bacteria cellulose is identical as the chemical structure of plant cellulose, accurately quantitative detection is thin
Retention of the fungin in paper is also rarely reported.
Summary of the invention
The purpose of the present invention is to provide a kind of sides of quantitative measurment bacteria cellulose retention in paper making process
Method reaches the efficient utilization to bacteria cellulose.
In order to achieve the above object, the technical solution adopted by the present invention is as follows.
A kind of method of quantitative measurment bacteria cellulose retention in paper making process, steps are as follows:
(1) bacterial cellulose wet-coating is cut into fritter, be added to the water, be separated into fine grained chippings using tissue mashing machine, with
It does not suspend still subject in water after standing a period of time.The sodium hydroxide solution for the use of mass fraction being 3~6% is to bacterial fibers
Element carries out swollen, uses magnetic stirrer sodium hydroxide-bacteria cellulose mixed liquor at normal temperature, and the bacterium in system is fine
The solid content of dimension element is 0.07~0.23%;
(2) in bacteria cellulose-caustic lye of soda that step (1) obtains, quaternary ammonium salt solution is added, makes itself and bacterium fibre
The molar ratio of glucose monomer in dimension element is that 1:1~5:1 is stirred under conditions of magnetic stirring apparatus is heated to 40~60 DEG C
Mix reaction 2~6 hours;
(3) solid-liquid mixing system that step (2) obtain is separated by solid-liquid separation using centrifuge, and uses mild acid wash mistake
The quaternary ammonium salt reagent and sodium hydroxide of amount, until the liquid portion isolated reaches neutral;
(4) the cationization bacteria cellulose with nitrogen label for obtaining step (3) is separated using tissue mashing machine
Until it becomes uniformly cotton-shaped, and the drying and forming-film on glass surface ware, taking weight is mbcSample analyzed using elemental analyser
Or x-ray photoelectron spectroscopy analysis, measure its nitrogen mass fraction Nbc;
(5) the cationization bacteria cellulose obtained in step (3) is separated using tissue mashing machine, and with dry weight percentage
Content 0.5~10% is blended with vegetable-fibre slurry, disperses fiber with bacteria cellulose using slurry fluffer and mixes
It is even, paper of manufacturing paper with pulp on paper making equipment;
(6) by after the paper manufactured paper with pulp in step (5) drying, taking weight is mpDo not have sample defective close to paper center,
Using elemental analyser, nitrogen mass fraction N is measuredp;
(7) pass through the mass fraction and step in conjunction with nitrogen in the cationization bacteria cellulose calculated in step (4)
Suddenly the mass fraction of nitrogen in the paper calculated in (6) calculates retention of the bacteria cellulose in paper making process, meter
It is as follows to calculate formula:
Wherein, R is retention %, mpFor the weight of paper, mbcFor the weight for the bacteria cellulose that is cationized, NpFor paper
The mass fraction of middle nitrogen, NbcFor the mass fraction of the nitrogen in cationization bacteria cellulose.
Further, the quaternary ammonium salt reagent refers to the cationic monomer containing ammonium, chloro base or epoxy group.
Further, the quaternary ammonium salt reagent is 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride, 2,3- glycidyl front three
One or more of ammonium chloride, 2,3- Epoxypropyl triethyl ammonium chloride and dimethyl dibenzyl ammonium chloride.
Further, bacteria cellulose described in step (1) is that bacterial micro-organism secretes synthesis under different condition of culture
Cellulose, English name Bacterial Cellulose (abbreviation BC), the bacteria cellulose is as paper making additive.
Further, the condition of culture is either statically or dynamically fermentation culture conditions.
Further, the bacterial micro-organism is glucose vinegar Bacillus (Gluconacetobacter), acetic acid Pseudomonas
(Acetobacter), Agrobacterium (Agrobacterium), pseudomonas (Pseudomonas), achromobacter
(Achrombacter), alcaligenes (Alcaligenes), Aerobacter (Aerobacter), azotobacter
(Azotobacter), one of rhizobium (Rhizabium) and Sarcina (Sarcina) or more.
Preferably, the bacterial micro-organism is in glucose vinegar Bacillus (Gluconacetobacter)
Gluconacetobacter europaeus,Gluconacetobacter intermedius,Gluconacetobacter
One or more of hansenii and Gluconacetobacter xylinus.
Further, the time of step (1) described stirring is 30min.
Further, the rate of step (3) described centrifuge is 5000rpm.
Further, step (5) vegetable-fibre slurry is that lumber fibre, non-wood plant fibre or secondary stock are logical
Cross the fibre stuff of mechanically or chemically pulp-making method preparation.
Further, the elemental analyser, which may also include, other can carry out quantitative analysis to the constituent content of material
Equipment.
Further, the equipment is x-ray photoelectron spectroscopy.
Further, step (5) the cationization bacteria cellulose is with dry weight percentage content 1~10% and plant fiber
Slurry is blended.
Further, step (4), step (5) the isolated time are 2 minutes.
Compared with prior art, the present invention has the advantage that elemental analyser is to the measurement sensitivity and standard of nitrogen
True rate is high, thus as paper making additive, the retention in paper in paper-making process quantifies bacteria cellulose provided by the invention
Detection method can achieve the Accurate Determining to retention.
Detailed description of the invention
Fig. 1 is a kind of process signal of quantitative measurment bacteria cellulose retention method in paper making process of the present invention
Figure.
Specific embodiment
Present invention is further described in detail by the following examples, but implementation of the invention is without being limited thereto.
Bacteria cellulose in embodiment is secreted by glucose vinegar bacillus (Glucoacetobacter xylinus).
The ingredient of bacteria culture media is main are as follows: ferment coconut water 50mL, ammonium sulfate 0.1g, magnesium sulfate 0.1g, potassium dihydrogen phosphate 0.1g, sugarcane
Sugared 3.0g, distilled water 50mL adjust pH value to 4.1,100 DEG C of sterilizing 5min with NaOH.Static fermentation cultural method: by culture medium
It is placed in 250mL beaker, is inoculated at 5% (V/V) glucose vinegar bacillus is 30 DEG C in temperature stationary culture 6 days.Dynamic fermentation training
Feeding method is to be inoculated with 5% (V/V) glucose vinegar bacillus in the medium, be placed in mechanical agitation type fermentor and cultivate 6 days, is sent out
Ferment condition is that 30 DEG C of temperature, ventilatory capacity 1.8L air/min/L and speed of agitator are 200r/min.The bacteria cellulose of acquisition
Solid content is about 1.5%.
The calculation formula of retention is as follows in embodiment:
Wherein, R is retention %, mpFor the weight of paper, mbcFor the weight for the bacteria cellulose that is cationized, NpFor paper
The mass fraction of middle nitrogen, NbcFor the mass fraction of the nitrogen in cationization bacteria cellulose.
Embodiment 1
It will be using the glucose vinegar bacillus (Glucoacetobacter xylinus) of dynamic fermentation training method culture point
The bacterial cellulose wet-coating 30g secreted is cut into fritter, is added in 100mL water, fine grained chippings is separated into using tissue mashing machine, with quiet
It does not suspend still subject in water after setting a period of time, adds the sodium hydroxide solution 100mL that mass fraction is 6%, make system
The solid content of bacteria cellulose reach 0.23%, use magnetic stirrer system 30min at normal temperature;3.58mL is added
3- chloro-2-hydroxypropyl-trimethyl ammonium chloride 65wt% aqueous solution, makes the molar ratio of itself and the glucose monomer in bacteria cellulose
It is stirred to react 6 hours under conditions of magnetic stirring apparatus is heated to 40 DEG C for 5:1;By system using centrifuge in 5000rpm
Under conditions of be separated by solid-liquid separation, and be added 200mL 0.005M hydrochloric acid solution cleaning cationization bacteria cellulose it is repeatedly straight
Reach neutral to the liquid portion being centrifugated out;The cationization bacteria cellulose marked with nitrogen is used into tissue mashing
Machine separate 2 minutes until it becomes uniformly it is cotton-shaped, be placed in drying and forming-film on glass surface ware, take cationization bacteria cellulose sample
Product 5mg is analyzed using elemental analyser, measures the mass fraction N of nitrogenbc;By the cationization bacteria cellulose of preparation
It is blended with dry weight percentage 10% with sugarcane fiber slurry (beating degree 240mL), using refiner by fiber and bacteria cellulose
It separates and is uniformly mixed under the conditions of 10000 turns/min, it is quantification of to control paper dry weight for paper of manufacturing paper with pulp on paper industry write by hand machine
1.4g/m2.It after drying, takes and does not have outturn 5mg defective close to paper center, using elemental analyser, measure nitrogen
Mass fraction Np.Using elemental analyser, the nitrogen mass fraction of cationization bacteria cellulose and composite paper is measured
Respectively 0.92% and 0.039%, finally calculating bacteria cellulose retention is 38.0%.
Embodiment 2
It will be using the glucose vinegar bacillus (Glucoacetobacter xylinus) of dynamic fermentation training method culture point
The bacterial cellulose wet-coating 20g secreted is cut into fritter, is added in 100mL water, fine grained chippings is separated into using tissue mashing machine, with quiet
It does not suspend still subject in water after setting a period of time, adds the sodium hydroxide solution 100mL that mass fraction is 4.5%, make body
The solid content of the bacteria cellulose of system reaches 0.15%, uses magnetic stirrer system 30min at normal temperature;It is added
0.48mL 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride 65wt% aqueous solution, makes itself and the glucose monomer in bacteria cellulose
Molar ratio is 1:1, under conditions of magnetic stirring apparatus is heated to 60 DEG C, is stirred to react 2 hours;System is existed using centrifuge
It is separated by solid-liquid separation under conditions of 5000rpm, and the hydrochloric acid solution cleaning cationization bacterial fibers of 200mL 0.005M is added
Element is repeatedly until the liquid portion being centrifugated out reaches neutral;The cationization bacteria cellulose marked with nitrogen is used
Tissue mashing machine separate 2 minutes until it becomes uniformly it is cotton-shaped, be placed in drying and forming-film on glass surface ware, take cationization bacterium
Cellulose sample 5mg is analyzed using elemental analyser, measures the mass fraction N of nitrogenbc;The cationization of preparation is thin
Fungin is blended with dry weight percentage 10% with sugarcane fiber slurry (beating degree 240mL), using refiner by fiber and carefully
Fungin is separated and is uniformly mixed under the conditions of 10000 turns/min, paper of manufacturing paper with pulp on paper industry write by hand machine, controls paper dry weight
Quantification of 1.4g/m2.It after drying, takes and does not have outturn 5mg defective close to paper center, use elemental analyser, measurement
Nitrogen mass fraction Np.Using elemental analyser, the nitrogen matter of cationization bacteria cellulose and composite paper is measured
Amount score is respectively 0.21% and 0.01%, and finally calculating bacteria cellulose retention is 42.9%.
Embodiment 3
It will be using the glucose vinegar bacillus (Glucoacetobacter xylinus) of static fermentation training method culture point
The bacterial cellulose wet-coating 10g secreted is cut into fritter, is added in 100mL water, fine grained chippings is separated into using tissue mashing machine, with quiet
It does not suspend still subject in water after setting a period of time, adds the sodium hydroxide solution 100mL that mass fraction is 3%, make system
The solid content of bacteria cellulose reach 0.075%, use magnetic stirrer system 30min at normal temperature;It is added
0.48mL 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride 65wt% aqueous solution, makes itself and the glucose monomer in bacteria cellulose
Molar ratio is 2:1, under conditions of magnetic stirring apparatus is heated to 50 DEG C, is stirred to react 4 hours;System is existed using centrifuge
It is separated by solid-liquid separation under conditions of 5000rpm, and the hydrochloric acid solution cleaning cationization bacterial fibers of 200mL 0.005M is added
Element is repeatedly until the liquid portion being centrifugated out reaches neutral;The cationization bacteria cellulose marked with nitrogen is used
Tissue mashing machine separate 2 minutes until it becomes uniformly it is cotton-shaped, be placed in drying and forming-film on glass surface ware, take cationization bacterium
Cellulose sample 5mg is analyzed using elemental analyser, measures the mass fraction N of nitrogenbc;The cationization of preparation is thin
Fungin is blended with dry weight percentage 5% with sugarcane fiber slurry (beating degree 240mL), using refiner by fiber and bacterium
Cellulose is separated and is uniformly mixed under the conditions of 10000 turns/min, paper of manufacturing paper with pulp on paper industry write by hand machine, and control paper dry weight is fixed
Amount is 1.4g/m2.It after drying, takes and does not have outturn 5mg defective close to paper center, using elemental analyser, measure nitrogen
Element mass fraction Np.Using elemental analyser, the nitrogen quality of cationization bacteria cellulose and composite paper is measured
Score is respectively 0.44% and 0.011%, and finally calculating bacteria cellulose retention is 47.5%.
Embodiment 4
It will be using the glucose vinegar bacillus (Glucoacetobacter xylinus) of static fermentation training method culture point
The bacterial cellulose wet-coating 10g secreted is cut into fritter, is added in 100mL water, fine grained chippings is separated into using tissue mashing machine, with quiet
It does not suspend still subject in water after setting a period of time, adds the sodium hydroxide solution 100mL that mass fraction is 3%, make system
The solid content of bacteria cellulose reach 0.075%, use magnetic stirrer system 30min at normal temperature;It is added
0.48mL 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride 65wt% aqueous solution, makes itself and the glucose monomer in bacteria cellulose
Molar ratio is 2:1, under conditions of magnetic stirring apparatus is heated to 50 DEG C, is stirred to react 4 hours;System is existed using centrifuge
It is separated by solid-liquid separation under conditions of 5000rpm, and the hydrochloric acid solution cleaning cationization bacterial fibers of 200mL 0.005M is added
Element is repeatedly until the liquid portion being centrifugated out reaches neutral;The cationization bacteria cellulose marked with nitrogen is used
Tissue mashing machine separate 2 minutes until it becomes uniformly it is cotton-shaped, be placed in drying and forming-film on glass surface ware, take cationization bacterium
Cellulose sample 5mg is analyzed using elemental analyser, measures the mass fraction N of nitrogenbc;The cationization of preparation is thin
Fungin is blended with dry weight percentage 1% with sugarcane fiber slurry (beating degree 240mL), using refiner by fiber and bacterium
Cellulose is separated and is uniformly mixed under the conditions of 10000 turns/min, paper of manufacturing paper with pulp on paper industry write by hand machine, and control paper dry weight is fixed
Amount is 1.4g/m2.It after drying, takes and does not have outturn 5mg defective close to paper center, using elemental analyser, measure nitrogen
Element mass fraction Np.Using elemental analyser, the nitrogen quality of cationization bacteria cellulose and composite paper is measured
Score is respectively 0.44% and 0.002%, and finally calculating bacteria cellulose retention is 50.9%.
Flow diagram of the invention is as shown in Figure 1.
The above enumerated are only specific embodiments of the present invention.Present invention is not limited to the above embodiments, can also there are many
Deformation.All deformations that those skilled in the art directly can export or associate from present disclosure, should all
It is considered protection scope of the present invention.
Claims (7)
1. a kind of method of quantitative measurment bacteria cellulose retention in paper making process, which is characterized in that including following
Step:
(1) bacterial cellulose wet-coating is separated into fine grained chippings using tissue mashing machine, the hydrogen-oxygen that mass fraction is 3~6% is added
Change sodium solution, so that the solid content of the bacteria cellulose of system is reached 0.07~0.23%, stirred at normal temperature using magnetic stirring apparatus
The system of mixing makes bacteria cellulose swollen, obtains bacteria cellulose-sodium hydroxide mixed liquor;
(2) in the bacteria cellulose that step (1) obtains-sodium hydroxide mixed liquor, quaternary ammonium salt solution is added, makes quaternary ammonium salt and thin
The molar ratio of glucose monomer in fungin is 1:1~5:1, under conditions of magnetic stirring apparatus is heated to 40~60 DEG C,
The reaction was stirred for 2 to 6 hours;The quaternary ammonium salt is 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride, 2,3- epoxypropyl trimethylammonium chloride
One or more of ammonium, 2,3- Epoxypropyl triethyl ammonium chloride and dimethyl dibenzyl ammonium chloride;
(3) solid-liquid mixing system that step (2) obtain is separated by solid-liquid separation using centrifuge, and mild acid wash solid sun is added
Ionization bacteria cellulose is repeatedly until the liquid being centrifugated out reaches neutral;
(4) by step (3) obtain with nitrogen label cationization bacteria cellulose using tissue mashing machine separate until
As uniformly it is cotton-shaped, be placed in drying and forming-film on glass surface ware, take weight be mbcSample penetrated using elemental analyser or X
Photoelectron Spectroscopy is analyzed, and the mass fraction N of nitrogen is measuredbc;
(5) the cationization bacteria cellulose with nitrogen label for obtaining step (3) is separated using tissue mashing machine, and with
Dry weight percentage 1~10% is blended with vegetable-fibre slurry, and fiber is dispersed and mixed with bacteria cellulose using slurry fluffer
It closes uniformly, paper of manufacturing paper with pulp on paper making equipment;
(6) by after the paper manufactured paper with pulp in step (5) drying, taking weight is mpDo not have sample defective close to paper center, uses member
Plain analyzer measures nitrogen mass fraction Np;
(7) pass through the mass fraction and step (6) in conjunction with nitrogen in the cationization bacteria cellulose calculated in step (4)
The mass fraction of nitrogen in the paper of middle calculating calculates retention of the bacteria cellulose in paper making process, calculates public
Formula is as follows:
Wherein, R is retention %, mpFor the weight of paper, mbcFor the weight for the bacteria cellulose that is cationized, NpFor nitrogen in paper
The mass fraction of element, NbcFor the mass fraction of the nitrogen in cationization bacteria cellulose.
2. a kind of method of quantitative measurment bacteria cellulose retention in paper making process according to claim 1,
It is characterized in that, bacteria cellulose described in step (1) is the fiber that bacterial micro-organism secretes synthesis under different condition of culture
Element.
3. a kind of method of quantitative measurment bacteria cellulose retention in paper making process according to claim 2,
It is characterized in that, the condition of culture is either statically or dynamically fermentation culture conditions.
4. a kind of method of quantitative measurment bacteria cellulose retention in paper making process according to claim 2,
It is characterized in that, the bacterial micro-organism is glucose vinegar Bacillus, acetic acid Pseudomonas, Agrobacterium, pseudomonas, nothing
One or more of Chromobacterium, alcaligenes, Aerobacter, azotobacter, rhizobium and Sarcina.
5. a kind of method of quantitative measurment bacteria cellulose retention in paper making process according to claim 1,
It is characterized in that, step (5) vegetable-fibre slurry is that lumber fibre, non-wood plant fibre or secondary stock pass through machinery
Or the fibre stuff of chemical pulping method preparation.
6. a kind of method of quantitative measurment bacteria cellulose retention in paper making process according to claim 1, feature
It is, the elemental analyser may also include other equipment that can carry out quantitative analysis to the constituent content of material.
7. according to a kind of method of quantitative measurment bacteria cellulose retention in paper making process of claim 6, feature
It is, the equipment is x-ray photoelectron spectroscopy.
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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 |
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