CN108458985A - A method of differentiating bamboo fibre - Google Patents
A method of differentiating bamboo fibre Download PDFInfo
- Publication number
- CN108458985A CN108458985A CN201810148943.7A CN201810148943A CN108458985A CN 108458985 A CN108458985 A CN 108458985A CN 201810148943 A CN201810148943 A CN 201810148943A CN 108458985 A CN108458985 A CN 108458985A
- Authority
- CN
- China
- Prior art keywords
- sample
- bamboo
- fiber
- fibre
- bamboo fibre
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 109
- 235000017166 Bambusa arundinacea Nutrition 0.000 title claims abstract description 73
- 235000017491 Bambusa tulda Nutrition 0.000 title claims abstract description 73
- 241001330002 Bambuseae Species 0.000 title claims abstract description 73
- 235000015334 Phyllostachys viridis Nutrition 0.000 title claims abstract description 73
- 239000011425 bamboo Substances 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 56
- 229920003043 Cellulose fiber Polymers 0.000 claims abstract description 25
- 239000007800 oxidant agent Substances 0.000 claims abstract description 20
- 230000003647 oxidation Effects 0.000 claims abstract description 19
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000012545 processing Methods 0.000 claims abstract description 13
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 11
- 238000001994 activation Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 229920000875 Dissolving pulp Polymers 0.000 claims abstract description 3
- 230000007935 neutral effect Effects 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000004570 mortar (masonry) Substances 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 10
- 238000001228 spectrum Methods 0.000 claims description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000013016 damping Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- DKNPRRRKHAEUMW-UHFFFAOYSA-N Iodine aqueous Chemical compound [K+].I[I-]I DKNPRRRKHAEUMW-UHFFFAOYSA-N 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 239000012047 saturated solution Substances 0.000 claims description 3
- 229910021583 Cobalt(III) fluoride Inorganic materials 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- WZJQNLGQTOCWDS-UHFFFAOYSA-K cobalt(iii) fluoride Chemical compound F[Co](F)F WZJQNLGQTOCWDS-UHFFFAOYSA-K 0.000 claims description 2
- 229910000464 lead oxide Inorganic materials 0.000 claims description 2
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims description 2
- KHIWWQKSHDUIBK-UHFFFAOYSA-N periodic acid Chemical compound OI(=O)(=O)=O KHIWWQKSHDUIBK-UHFFFAOYSA-N 0.000 claims description 2
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 2
- 239000012286 potassium permanganate Substances 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 239000005708 Sodium hypochlorite Substances 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 125000001309 chloro group Chemical group Cl* 0.000 claims 1
- 238000000227 grinding Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims 1
- 238000005303 weighing Methods 0.000 claims 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 abstract description 13
- 150000004056 anthraquinones Chemical class 0.000 abstract description 13
- 229920000297 Rayon Polymers 0.000 description 9
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 7
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011978 dissolution method Methods 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000012850 discrimination method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 102000008946 Fibrinogen Human genes 0.000 description 1
- 108010049003 Fibrinogen Proteins 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- RGHILYZRVFRRNK-UHFFFAOYSA-N anthracene-1,2-dione Chemical compound C1=CC=C2C=C(C(C(=O)C=C3)=O)C3=CC2=C1 RGHILYZRVFRRNK-UHFFFAOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229940012952 fibrinogen Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- PNYYBUOBTVHFDN-UHFFFAOYSA-N sodium bismuthate Chemical compound [Na+].[O-][Bi](=O)=O PNYYBUOBTVHFDN-UHFFFAOYSA-N 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- 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
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
Landscapes
- 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)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The present invention relates to a kind of methods differentiating bamboo fibre, including：(1) by cellulose fibre sample aqueous slkali activation process to be measured, treatment temperature is 25 95 DEG C, and processing time is 0.1 4h, bath raio 1:20 60, it is separated by filtration, is washed to neutral, drying, obtain activated sample；(2) the activated sample strong oxidizer for not dissolving cellulose fibre is handled, treatment temperature is 25 95 DEG C, and processing time is 0.1 4h, bath raio 1:20 60, obtain sample after oxidation processes；(3) examination of infrared spectrum is carried out after coupons being made in the sample after oxidation processes, is differentiated by sample infrared spectrogram.The present invention provides a kind of method of the discriminating bamboo fibre carried out for the important component anthraquinone in bamboo fibre, this method is sensitive and accurate.
Description
Technical field
The invention belongs to cellulose fibre authentication technique field, more particularly to a kind of method differentiating bamboo fibre.
Background technology
Bamboo fibre is a kind of novel biomass fiber.Studies have shown that bamboo fibre and its product naturally have antibacterial bacteriostatic etc.
Other unexistent excellent properties of cellulose fibre.Different according to selection and processing technology, bamboo fibre is divided into bamboo fiber and bamboo
Two class of pulp fibres.Bamboo fiber is the bast fiber obtained from bamboo stem, is a kind of primary fibre directly extracted from bamboo pole
Dimension.Bamboo pulp fiber is that pulp, then the regenerated celulose fibre made of viscose rayon spinning technique is made in bamboo wood.Due to bamboo
There are larger differences in price for fibrinogen, bamboo pulp fiber and common viscose fiber, drive businessman by common viscose fiber mark
Note is bamboo fibre, is adulterated.It does so and has both led consumer into a trap, also affect the sustainable development of bamboo fibre industry.One
The sound development of industry be unable to do without standard working-out and is innovated with detection method, wherein important one be exactly formulate as early as possible bamboo fibre with
The discrimination method that viscose rayon strictly distinguishes.
Have at present about the patent for preparing bamboo fibre it is many, such as ZL 20081017872.2 " complex function type bamboo
The Chinese patent etc. of pulp fibres and preparation method thereof ".But the patent about discriminating bamboo fibre is seldom, ZL
The Chinese patent of 200810034237.6 " a method of with dissolution method differentiate bamboo pulp fiber ", which discloses, a kind of using dissolution method
Differentiate the method for bamboo pulp fiber.
Differentiate that the method for bamboo fibre has combustion method, microscopic observation, coloring medicine method, infra-red sepectrometry, density gradient
Method and dissolution method etc..These methods are carried out for the main component cellulose in bamboo fibre.
Invention content
Technical problem to be solved by the invention is to provide a kind of methods differentiating bamboo fibre, and the present invention provides a kind of needles
The new method for the discriminating bamboo fibre that important component anthraquinone in bamboo fibre is carried out.
A kind of method of discriminating bamboo fibre of the present invention, including：
(1) by cellulose fibre sample aqueous slkali activation process to be measured, treatment temperature is 25-95 DEG C, and processing time is
0.1-4h, bath raio 1:20-60 is separated by filtration, is washed to neutral, drying, obtains activated sample；The wherein concentration of aqueous slkali
For 5-25wt%；
(2) activated sample for obtaining step (1) is handled with the strong oxidizer for not dissolving cellulose fibre, and treatment temperature is
25-95 DEG C, processing time 0.1-4h, bath raio 1:20-60 obtains sample after oxidation processes；Wherein insoluble cellulose fiber
The strong oxidizer content of dimension is 1-10g/L；
(3) examination of infrared spectrum is carried out after coupons being made in sample after oxidation processes that step (2) obtains, passes through sample
Infrared spectrogram differentiates；Wherein 3450-3200cm in the infrared spectrogram of coupons-1、1640cm-1、1160cm-1、1064-
980cm-1、893cm-1、671-667cm-1、610cm-1Place is without characteristic peak, then fiber undetermined does not belong to cellulose fibre；Coupons
Infrared spectrogram on remove 3450cm-1、1640cm-1、1060cm-1Place is outer, in 1710cm-1Nearby also there is characteristic peak at place, then
Fiber category bamboo fibre undetermined；If 3450cm in the infrared spectrogram of coupons-1、1640cm-1、1060cm-1Nearby there is spy at place
Sign absorption peak, and 1710cm-1Place or nearby without characteristic peak, then other cellulose fibres of the fiber category undetermined in addition to bamboo fibre.
Aqueous slkali in the step (1) is sodium hydroxide solution.
The strong oxidizer of insoluble cellulose fibre in the step (2) is chlorine, potassium permanganate, potassium bichromate, secondary
One or more of sodium chlorate, hydrogen peroxide, brown lead oxide, sodium bismuthate, periodic acid, cobalt trifluoride, Na2Fe04.
In the step (3) by the sample after oxidation processes be made coupons the specific steps are：Powder in the agate mortar
The KBr of the broken order of spectrum is simultaneously ground to fine powder, is put in drying in vacuum drying oven, is placed in drier for use；After oxidation processes
Sample is washed to neutrality, is placed in vacuum drying oven and dries 8-24h to over dry；Weigh the fiber sample drying of 0.5-2.5mg, damping
It is finely ground to 2 μ after 16-24h；The fiber sample of 1-2mg is weighed, and with 1mg samples 100-200mgKBr ratios are weighed dry
KBr is ground in drying box in the agate mortar together, until the two is mixed thoroughly；It is uniform to weigh 200mg
Mixture is poured into the mould that pressed disc method uses, and a diameter of 10-13mm is made, the thin slice that thickness is 0.5-0.8mm.
Bamboo fibre in the step (3) is bamboo pulp fiber or bamboo fiber.
Coupons are accredited as bamboo fibre in the step (3), and then fiber is placed in iodine-potassium iodide saturated solution, punching
It washes that dry rear fiber uncolored, is bamboo pulp fiber.
Using anthraquinone, its carbonyl under the action of strong oxidizer is oxidized to-COOH to the present invention, and-COOH is in infrared spectrum
1710cm on figure-1Nearby there is the characteristics of characteristic peak at place, and infra-red sepectrometry is used after fiber to be measured is handled with strong oxidizer
To differentiate.This method is sensitive and accurate, is conducive to strictly distinguish bamboo fibre and viscose rayon and other cellulose fibres.But current portion
Divide bamboo fibre, especially by bamboo pulp fiber made of viscose rayon spinning technique, anthraquinone content is few, and the chemistry knot of the fiber
Structure is complicated, crystallinity is high, and strong oxidizer is low with the accessibility of anthraquinone, therefore cannot efficiently generate certain amount in infrared spectrum
1710cm on figure-1Place or the-COOH for nearby having characteristic peak.Therefore the present invention first leads to sample to be tested before bamboo fibre is aoxidized
It crosses alkali process to be activated, to improve the accessibility of strong oxidizer and anthraquinone, realization more accurately differentiates.
Advantageous effect
(1) differentiate that the method for bamboo fibre is carried out for the main component cellulose in bamboo fibre in the prior art,
The present invention provides a kind of new methods of the discriminating bamboo fibre carried out for the important component anthraquinone in bamboo fibre；
(2) present invention activates bamboo fibre by alkali process, makes strong oxidizer when anthraquinone content is less in bamboo fibre
It can react with anthraquinone, and the condition for making anthraquinone its carbonyl under the action of strong oxidizer be oxidized to-COOH is broader,
It is more advantageous to the accurate discriminating of bamboo fibre；
(3) present invention is oxidized to-COOH using anthraquinone its carbonyl under the action of strong oxidizer, and-COOH is infrared
1710cm on spectrogram-1Nearby there is the characteristics of characteristic peak at place, and infrared light is used after fiber to be measured is handled with strong oxidizer
Spectrometry differentiates；
(4) discrimination method of the invention is more sensitive and accurate, is conducive to strictly to distinguish bamboo fibre and viscose rayon and other
Cellulose fibre.
Description of the drawings
Fig. 1 is the infrared spectrogram of bamboo fibre in embodiment 1；
Fig. 2 is the infrared spectrogram of viscose rayon in embodiment 2；
Fig. 3 is the infrared spectrogram of bamboo fibre in comparative example 1.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
(1) by the sodium hydroxide solution activation process of a concentration of 20wt% of cellulose fibre sample to be measured, treatment temperature
It is 25 DEG C, processing time 2h, bath raio 1:30, it is separated by filtration, is fully washed to neutrality, then 105 with deionized water
Dry 12h, obtains activated sample, is sealed spare at DEG C.
(2) strong oxidizer pair for the insoluble cellulose fibre for being 5g/L with content by the activated sample that step (1) obtains
Oxygen water process, treatment temperature are 50 DEG C, processing time 1h, bath raio 1:45, obtain sample after oxidation processes.
(3) coupons are made in sample after oxidation processes that step (2) obtains, crush the order of spectrum in the agate mortar
KBr is simultaneously ground to fine powder, is put in drying in vacuum drying oven, is placed in drier for use；The sample after oxidation processes with 80 DEG C
It is washed to neutrality, is placed in vacuum drying oven and dries 16h to over dry；The fiber sample drying of 2mg is weighed, it is finely ground to 2 μ after damping for 24 hours；
The fiber sample of 2mg is weighed, and dry KBr is weighed to 150mgKBr ratios with 1mg samples and is existed in the agate mortar together
It is ground in drying box, until the two is mixed thoroughly；The uniform mixtures of 200mg are weighed, pressed disc method is carefully poured into
In the mould used, a diameter of 13mm is made, the transparent sheet that thickness is 0.8mm.
(4) infrared spectrogram for the coupons that determination step (3) obtains on infrared spectrometer：Open infrared spectrometer
Power supply opens lid, the sample made is fixed on holder after its stabilization；Run spectrometer monitoring programme；Setting test
Parameter：Instrumental resolution is 4cm-1；Sweep speed is 0.2cm/s；Scanning times are 32 times；Wave number scanning range be 400~
4000cm-1；After the completion of parameter setting, background scans are carried out；It waits for carrying out coupons scanning after the completion of background scans；After the completion of scanning
Infrared spectrum is obtained as shown in Figure 1, characteristic peak on analysis of spectra, finds 3296.05cm-1、1713.42cm-1、1644.52cm-1、1713.42cm-1There is characteristic peak at place, judges fiber category bamboo fibre to be measured, and 2g fibers are further placed on iodine-potassium iodide saturation
In solution, it is uncolored that rear fiber is dried in flushing, therefore, it is determined that fiber to be measured is bamboo pulp fiber.
Embodiment 2
(1) by the sodium hydroxide solution activation process of a concentration of 20wt% of cellulose fibre sample to be measured, treatment temperature
It is 25 DEG C, processing time 2h, bath raio 1:30, it is separated by filtration, is fully washed to neutrality, then 105 with deionized water
Dry 12h, obtains activated sample, is sealed spare at DEG C.
(2) strong oxidizer pair for the insoluble cellulose fibre for being 5g/L with content by the activated sample that step (1) obtains
Oxygen water process, treatment temperature are 50 DEG C, processing time 1h, bath raio 1:45, obtain sample after oxidation processes.
(3) coupons are made in sample after oxidation processes that step (2) obtains, crush the order of spectrum in the agate mortar
KBr is simultaneously ground to fine powder, is put in drying in vacuum drying oven, is placed in drier for use；The sample after oxidation processes with 80 DEG C
It is washed to neutrality, is placed in vacuum drying oven and dries 16h to over dry；The fiber sample drying of 2mg is weighed, it is finely ground to 2 μ after damping for 24 hours；
The fiber sample of 2mg is weighed, and dry KBr is weighed to 150mgKBr ratios with 1mg samples and is existed in the agate mortar together
It is ground in drying box, until the two is mixed thoroughly；The uniform mixtures of 200mg are weighed, pressed disc method is carefully poured into
In the mould used, a diameter of 13mm is made, the transparent sheet that thickness is 0.8mm.
(4) infrared spectrogram for the coupons that determination step (3) obtains on infrared spectrometer：Open infrared spectrometer
Power supply opens lid, the sample made is fixed on holder after its stabilization；Run spectrometer monitoring programme；Setting test
Parameter：Instrumental resolution is 4cm-1；Sweep speed is 0.2cm/s；Scanning times are 32 times；Wave number scanning range be 400~
4000cm-1；After the completion of parameter setting, background scans are carried out；It waits for carrying out coupons scanning after the completion of background scans；After the completion of scanning
Infrared spectrum is obtained as shown in Fig. 2, characteristic peak on analysis of spectra, finds 3450cm-1、1640cm-1、1060cm-1Place nearby has
Characteristic peak, 1710cm-1Place judges other cellulose fibres of the fiber category to be measured in addition to bamboo fibre, further nearby without characteristic peak
Fibre morphology is observed by microscopic method, discovery fibre section is sawtooth pattern, therefore, it is determined that fiber to be measured is viscose rayon.
Comparative example 1
(1) the strong oxidizer hydrogen peroxide for the insoluble cellulose fibre for being 5g/L with content by cellulose fibre sample to be measured
Processing, treatment temperature are 50 DEG C, processing time 1h, bath raio 1:45, obtain sample after oxidation processes.
(2) coupons are made in sample after oxidation processes that step (1) obtains, crush the order of spectrum in the agate mortar
KBr is simultaneously ground to fine powder, is put in drying in vacuum drying oven, is placed in drier for use；The sample after oxidation processes with 80 DEG C
It is washed to neutrality, is placed in vacuum drying oven and dries 16h to over dry；The fiber sample drying of 2mg is weighed, it is finely ground to 2 μ after damping for 24 hours；
The fiber sample of 2mg is weighed, and dry KBr is weighed to 150mgKBr ratios with 1mg samples and is existed in the agate mortar together
It is ground in drying box, until the two is mixed thoroughly；The uniform mixtures of 200mg are weighed, pressed disc method is carefully poured into
In the mould used, a diameter of 13mm is made, the transparent sheet that thickness is 0.8mm.
(4) infrared spectrogram for the coupons that determination step (2) obtains on infrared spectrometer：Open infrared spectrometer
Power supply opens lid, the sample made is fixed on holder after its stabilization；Run spectrometer monitoring programme；Setting test
Parameter：Instrumental resolution is 4cm-1；Sweep speed is 0.2cm/s；Scanning times are 32 times；Wave number scanning range be 400~
4000cm-1；After the completion of parameter setting, background scans are carried out；It waits for carrying out coupons scanning after the completion of background scans；After the completion of scanning
Infrared spectrum is obtained as shown in fig. 3, it was found that 3450cm-1、1640cm-1、1060cm-1、1710cm-1Nearby there is characteristic peak at place, judges
2g fibers, are further placed in iodine-potassium iodide saturated solution by fiber category bamboo fibre to be measured, and it is uncolored that rear fiber is dried in flushing,
Therefore, it is determined that fiber to be measured is bamboo pulp fiber.
The cellulose fibre sample infrared spectrum that this comparative example and embodiment 1 obtain is compared it is found that activated place
The infrared spectrum that the cellulose fibre sample of reason obtains is compared with the infrared spectrum that the cellulose fibre sample without activation process obtains
More precisely, it also turns out the alkali process activation in the present invention, makes strong oxidizer when anthraquinone content is less in bamboo fibre also can be with anthracene
Quinone reacts, and the condition for making anthraquinone its carbonyl under the action of strong oxidizer be oxidized to-COOH is broader, to real
Existing bamboo fibre more accurately differentiates.
Claims (6)
1. a kind of method differentiating bamboo fibre, including：
(1) by cellulose fibre sample aqueous slkali activation process to be measured, treatment temperature is 25-95 DEG C, processing time 0.1-
4h, bath raio 1:20-60 is separated by filtration, is washed to neutral, drying, obtains activated sample；The wherein a concentration of 5- of aqueous slkali
25wt%；
(2) activated sample for obtaining step (1) is handled with the strong oxidizer for not dissolving cellulose fibre, treatment temperature 25-
95 DEG C, processing time 0.1-4h, bath raio 1:20-60 obtains sample after oxidation processes；Wherein insoluble cellulose fibre
Strong oxidizer content is 1-10g/L；
(3) sample after oxidation processes that step (2) obtains is made after coupons and carries out examination of infrared spectrum, it is infrared by sample
Spectrogram differentiates；Wherein 3450-3200cm in the infrared spectrogram of coupons-1、1640cm-1、1160cm-1、1064-980cm-1、
893cm-1、671-667cm-1、610cm-1Place is without characteristic peak, then fiber undetermined does not belong to cellulose fibre；The infrared light of coupons
3450cm is removed on spectrogram-1、1640cm-1、1060cm-1Place is outer, in 1710cm-1Nearby also there is characteristic peak at place, then fiber undetermined
Belong to bamboo fibre；If 3450cm in the infrared spectrogram of coupons-1、1640cm-1、1060cm-1Nearby there is characteristic absorption at place
Peak, and 1710cm-1Place or nearby without characteristic peak, then other cellulose fibres of the fiber category undetermined in addition to bamboo fibre.
2. a kind of method differentiating bamboo fibre according to claim 1, it is characterised in that：Alkali soluble in the step (1)
Liquid is sodium hydroxide solution.
3. a kind of method differentiating bamboo fibre according to claim 1, it is characterised in that：It is insoluble in the step (2)
The strong oxidizer for solving cellulose fibre is chlorine, potassium permanganate, potassium bichromate, sodium hypochlorite, hydrogen peroxide, brown lead oxide, bismuthic acid
One or more of sodium, periodic acid, cobalt trifluoride, Na2Fe04.
4. a kind of method differentiating bamboo fibre according to claim 1, it is characterised in that：It will oxidation in the step (3)
Sample is made coupons that treated the specific steps are：The KBr of the order of spectrum is crushed in the agate mortar and is ground to fine powder, is put
It is dry in vacuum drying oven, it is placed in drier for use；Sample after oxidation processes is washed to neutrality, is placed in vacuum drying oven
8-24h is dried to over dry；The fiber sample for weighing 0.5-2.5mg is dried, finely ground to 2 μ after damping 16-24h；Weigh the fibre of 1-2mg
It ties up sample, and dry KBr is weighed together in the agate mortar in drying box to 100-200mgKBr ratios with 1mg samples
Grinding, until the two is mixed thoroughly；The uniform mixtures of 200mg are weighed, are poured into the mould that pressed disc method uses,
A diameter of 10-13mm is made, the thin slice that thickness is 0.5-0.8mm.
5. a kind of method differentiating bamboo fibre according to claim 1, it is characterised in that：Bamboo in the step (3) is fine
Dimension is bamboo pulp fiber or bamboo fiber.
6. a kind of method differentiating bamboo fibre according to claim 1, it is characterised in that：Coupons in the step (3)
It is accredited as bamboo fibre, then fiber is placed in iodine-potassium iodide saturated solution, it is uncolored that rear fiber is dried in flushing, is that bamboo pulp is fine
Dimension.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810148943.7A CN108458985A (en) | 2018-02-13 | 2018-02-13 | A method of differentiating bamboo fibre |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810148943.7A CN108458985A (en) | 2018-02-13 | 2018-02-13 | A method of differentiating bamboo fibre |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108458985A true CN108458985A (en) | 2018-08-28 |
Family
ID=63216502
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810148943.7A Pending CN108458985A (en) | 2018-02-13 | 2018-02-13 | A method of differentiating bamboo fibre |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108458985A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102661929A (en) * | 2012-03-12 | 2012-09-12 | 中国林业科学研究院木材工业研究所 | Identification method of bamboo raw fiber based on infrared and two-dimensional correlation spectra |
| CN104390929A (en) * | 2014-10-29 | 2015-03-04 | 东华大学 | Method for identifying bamboo fibers |
| CN106226258A (en) * | 2016-08-10 | 2016-12-14 | 四川大学 | A kind of method differentiating bamboo pulp fiber and common viscose fiber |
| CN107141513A (en) * | 2017-05-18 | 2017-09-08 | 宿州市逢源生物科技有限公司 | A kind of degradable liquid ground film solution of bamboo fiber-based water conservation and preparation method thereof |
| CN107523984A (en) * | 2017-09-25 | 2017-12-29 | 安徽华祺汽车装饰有限公司 | A kind of production method of bamboo fibre |
-
2018
- 2018-02-13 CN CN201810148943.7A patent/CN108458985A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102661929A (en) * | 2012-03-12 | 2012-09-12 | 中国林业科学研究院木材工业研究所 | Identification method of bamboo raw fiber based on infrared and two-dimensional correlation spectra |
| CN104390929A (en) * | 2014-10-29 | 2015-03-04 | 东华大学 | Method for identifying bamboo fibers |
| CN106226258A (en) * | 2016-08-10 | 2016-12-14 | 四川大学 | A kind of method differentiating bamboo pulp fiber and common viscose fiber |
| CN107141513A (en) * | 2017-05-18 | 2017-09-08 | 宿州市逢源生物科技有限公司 | A kind of degradable liquid ground film solution of bamboo fiber-based water conservation and preparation method thereof |
| CN107523984A (en) * | 2017-09-25 | 2017-12-29 | 安徽华祺汽车装饰有限公司 | A kind of production method of bamboo fibre |
Non-Patent Citations (5)
| Title |
|---|
| BALAJI A.N.等: "Characterization of alkali treated and untreated new cellulosic fiber from Saharan aloe vera cactus leaves", 《CARBOHYDRATE POLYMERS》 * |
| 唐人成等: "松式碱处理对竹纤维直接染料染色性能的影响", 《印染》 * |
| 王敬尊等: "《复杂样品的综合分析—剖析技术概论》", 30 September 2000, 化学工业出版社 * |
| 裴月湖等: "《有机化合物波谱解析》", 31 August 2015, 中国医药科技出版社 * |
| 赵嘉等: "活化处理对竹纤维结构和性能的影响", 《化工新型材料》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Hurtubise et al. | Classification of fine structural characteristics in cellulose by infared spectroscopy. Use of potassium bromide pellet technique | |
| Schenzel et al. | NIR FT Raman spectroscopy–a rapid analytical tool for detecting the transformation of cellulose polymorphs | |
| Tian et al. | Improvement in the Fock test for determining the reactivity of dissolving pulp | |
| CN103554274B (en) | A kind of preparation method of sugarcane marrow SURGICEL | |
| JP2020034565A (en) | Fiber identification method | |
| CN108458985A (en) | A method of differentiating bamboo fibre | |
| CN104655580B (en) | A kind of method of the chemical cellulose content in quick measure dissolving pulp | |
| CN108645811A (en) | A method of Chinese herbal medicine Radix Notoginseng is detected using Terahertz Technology | |
| Huang et al. | Anthraquinone-assisted deep eutectic solvent degumming of ramie fibers: evaluation of fiber properties and degumming performance | |
| CN108827907A (en) | It is a kind of based near infrared spectrum to the rapid assay methods of color cotton coloration | |
| JP6771576B2 (en) | Fiber identification method | |
| CN102426147A (en) | Method for distinguishing Lyocell bamboo fiber in blending product | |
| Bhattacharya et al. | Alkali degumming of decorticated ramie | |
| CN104390929A (en) | Method for identifying bamboo fibers | |
| CN104931322B (en) | A kind of quantitative analysis method of cotton and viscose blend fabric | |
| CN101251530B (en) | Method for identification of bamboo pulp fiber by dissolution method | |
| Gong et al. | Natural colorant extraction from Cinnamomum camphora tree leaves of different maturities and its ultrasonic‐assisted extraction process | |
| Ranby | The mercerisation of cellulose | |
| CN110230111A (en) | A method of Lyocell fibers are prepared by raw material of poplar | |
| Macmillan et al. | 30—THE DETECTION AND ESTIMATION OF DAMAGE IN JUTE FIBRE Part I—A NEW MICROSCOPICAL TEST AND THE IMPLICATIONS OF CERTAIN CHEMICAL TESTS | |
| CN106226258B (en) | A method of differentiating bamboo pulp fiber and common viscose fiber | |
| US4689045A (en) | Procedure for the preparation of modified cellulose | |
| CN111537494A (en) | Analysis method for furfural extraction effect in transformer oil | |
| Yonenobu et al. | Non-destructive near infrared spectroscopic measurement of antique washi calligraphic scrolls | |
| Dass et al. | Extraction and Testing of Natural Dye from Dafara (Cissus populnea) Stem Bark and Its Application on Cotton Fabric |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180828 |