CN106368027A - Method for preparing nanocellulose through oxidative degradation of ammonium persulfate - Google Patents
Method for preparing nanocellulose through oxidative degradation of ammonium persulfate Download PDFInfo
- Publication number
- CN106368027A CN106368027A CN201611012126.6A CN201611012126A CN106368027A CN 106368027 A CN106368027 A CN 106368027A CN 201611012126 A CN201611012126 A CN 201611012126A CN 106368027 A CN106368027 A CN 106368027A
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- CN
- China
- Prior art keywords
- ammonium persulfate
- cellulose
- distilled water
- nano
- oxidation degradation
- 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.)
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Classifications
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21B1/00—Fibrous raw materials or their mechanical treatment
- D21B1/02—Pretreatment of the raw materials by chemical or physical means
- D21B1/021—Pretreatment of the raw materials by chemical or physical means by chemical means
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21B1/00—Fibrous raw materials or their mechanical treatment
- D21B1/04—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres
- D21B1/12—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres by wet methods, by the use of steam
- D21B1/30—Defibrating by other means
- D21B1/306—Defibrating by other means using microwaves
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C1/00—Pretreatment of the finely-divided materials before digesting
- D21C1/06—Pretreatment of the finely-divided materials before digesting with alkaline reacting compounds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a method for preparing nanocellulose through oxidative degradation of ammonium persulfate. The method includes the following steps that 1, paper pulp is added into an ammonium persulfate solution, the mixture is stirred for 16 h at the constant temperature of 70 DEG C at constant speed, then distilled water is added for dilution, and a reaction is ended; 2, standing is carried out for 24 h, supernatant liquid is removed, a high-speed freezing centrifuge is utilized for centrifuging suspension liquid, supernatant liquid is removed after centrifuging is carried out each time, and distilled water is added for dilution until the supernatant liquid becomes turbid; 3, the turbid liquid is collected into a dialysis bag and dialyzed for 2-3 d in flowing distilled water until the pH value ranges from 6 to 7, and the nanocellulose is prepared after ultrasonic dispersing treatment. The method is easy to operate, has the mild reaction, and is low in energy consumption, small in water consumption and environmentally friendly, products are easy to separate, the prepared nanocellulose product is good in performance and large in length-diameter ratio, and the diameter uniformly ranges from 35 nm to 50 nm.
Description
Technical field
The invention belongs to the preparation field of nano-cellulose is and in particular to a kind of Ammonium persulfate. oxidation degradation method prepares nanometer
The method of cellulose.
Background technology
Cellulose is reserves natural polymer the abundantest in nature, has low cost, renewable and can
The good characteristics such as biodegradation.With the development of nanotechnology, separate nano-cellulose from biological material, prepare nanoscale
Other cellulosic material, has the advantages that compared with traditional cellulosic material specific surface area is big, intensity is high, heat stability good.
Additionally, nano-cellulose surface exposes more hydroxyls and reducing end group can make cellulose surface grafting chemical functional group change
Property, this provides for its replacement conventional synthesis macromolecule may be so as to be applied more broadly in biomedicine, pharmacy and function
The fields such as material.
The common preparation method of nano-cellulose have chemical method, Mechanical Method, bioanalysises, synthetic method, electrostatic weaving and
Ferment treatment method.Acid hydrolyzation is prepared nano-cellulose and is used the strong sulphuric acid hydrolysis cellulose of corrosivity, and hydrolysis is violent, effect on environment
Greatly, and acid hydrolyzation prepares that nano-cellulose yield is low, water consumption big, and consersion unit is required higher.Mechanical Method preparation is received
Rice cellulose power consumption is big, and effective utilization rate of energy is relatively low.Therefore, develop the new efficient, environmental friendliness of nano-cellulose, can
Control, low energy consumption preparation method particularly important.
Content of the invention
The present invention provides a kind of method that Ammonium persulfate. oxidation degradation method prepares nano-cellulose, and energy consumption is low, has environment
Friendly.
The present invention is achieved by the following technical solutions.
A kind of method that Ammonium persulfate. oxidation degradation method prepares nano-cellulose, comprises the following steps:
(1) paper pulp is added in ammonium persulfate solution, 70 DEG C of constant temperature constant speed add distilled water diluting after stirring 16 h and terminate
Reaction；
(2) stand 24h, remove the supernatant, using High speed refrigerated centrifuge, suspension is centrifuged, after being centrifuged every time, remove upper strata
Clear liquid, and add distilled water diluting, until supernatant becomes cloudy；
(3) turbid solution is collected in bag filter, dialyse in the distilled water of flowing 2-3 d, until ph 6～7, carries out ultrasonic
Decentralized processing, prepared nano-cellulose.
Preferably, in above-mentioned steps (1), paper pulp, Ammonium persulfate., the mass ratio of distilled water are: 1:100:200.
Preferably, in above-mentioned steps (1), the concentration of Ammonium persulfate. is 1.5mol/l.
Preferably, in above-mentioned steps (2), the rotating speed of centrifugally operated is 21000 r/min, and centrifugation time is 10 min.
Preferably, in above-mentioned steps (3), the power of ultrasonic disperse is 2000 w, and ultrasonic time is 20min.
Advantages of the present invention:
The present invention prepares nano-cellulose using Ammonium persulfate. oxidation degradation method, simple to operate, and reaction is relatively gentle, energy consumption is low,
Water consumption is little, has environment friendly, and product is easily separated, the nano-cellulose good product performance of preparation, and draw ratio is big, and diameter divides
Cloth is in 35-50nm, distribution uniform.
Specific embodiment
Embodiment 1
A kind of method that Ammonium persulfate. oxidation degradation method prepares nano-cellulose, comprises the following steps:
(1) paper pulp is added in ammonium persulfate solution, 70 DEG C of constant temperature constant speed add distilled water diluting after stirring 16 h and terminate
Reaction；
(2) stand 24h, remove the supernatant, using High speed refrigerated centrifuge, suspension is centrifuged, after being centrifuged every time, remove upper strata
Clear liquid, and add distilled water diluting, until supernatant becomes cloudy；
(3) turbid solution is collected in bag filter, dialyse in the distilled water of flowing 2-3 d, until ph 6～7, carries out ultrasonic
Decentralized processing, prepared nano-cellulose.
Embodiment 2
A kind of method that Ammonium persulfate. oxidation degradation method prepares nano-cellulose, comprises the following steps:
(1) paper pulp is added in ammonium persulfate solution, 70 DEG C of constant temperature constant speed add distilled water diluting after stirring 16 h and terminate
Reaction, wherein, paper pulp, Ammonium persulfate., the mass ratio of distilled water are: 1:100:200, and the concentration of Ammonium persulfate. is 1.5mol/l；
(2) stand 24h, remove the supernatant, using High speed refrigerated centrifuge, suspension is centrifuged, the rotating speed of centrifugally operated is
21000 r/min, centrifugation time is 10 min, removes the supernatant, and add distilled water diluting after being centrifuged every time, until supernatant
Liquid becomes cloudy；
(3) turbid solution is collected in bag filter, dialyse in the distilled water of flowing 2-3 d, until ph 6～7, carries out ultrasonic
Decentralized processing, the power of ultrasonic disperse is 2000 w, and ultrasonic time is 20min, prepared nano-cellulose.
Claims (5)
1. a kind of Ammonium persulfate. oxidation degradation method prepare nano-cellulose method it is characterised in that: comprise the following steps:
(1) paper pulp is added in ammonium persulfate solution, 70 DEG C of constant temperature constant speed add distilled water diluting after stirring 16 h and terminate
Reaction；
(2) stand 24h, remove the supernatant, using High speed refrigerated centrifuge, suspension is centrifuged, after being centrifuged every time, remove upper strata
Clear liquid, and add distilled water diluting, until supernatant becomes cloudy；
(3) turbid solution is collected in bag filter, dialyse in the distilled water of flowing 2-3 d, until ph 6～7, carries out ultrasonic
Decentralized processing, prepared nano-cellulose.
2. the method that a kind of Ammonium persulfate. oxidation degradation method according to claim 1 prepares nano-cellulose, its feature exists
In: in step (1), paper pulp, Ammonium persulfate., the mass ratio of distilled water are: 1:100:200.
3. the method that a kind of Ammonium persulfate. oxidation degradation method according to claim 1 prepares nano-cellulose, its feature exists
In: in step (1), the concentration of Ammonium persulfate. is 1.5mol/l.
4. the method that a kind of Ammonium persulfate. oxidation degradation method according to claim 1 prepares nano-cellulose, its feature exists
In: in step (2), the rotating speed of centrifugally operated is 21000 r/min, and centrifugation time is 10 min.
5. the method that a kind of Ammonium persulfate. oxidation degradation method according to claim 1 prepares nano-cellulose, its feature exists
In: in step (3), the power of ultrasonic disperse is 2000 w, and ultrasonic time is 20min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611012126.6A CN106368027A (en) | 2016-11-17 | 2016-11-17 | Method for preparing nanocellulose through oxidative degradation of ammonium persulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611012126.6A CN106368027A (en) | 2016-11-17 | 2016-11-17 | Method for preparing nanocellulose through oxidative degradation of ammonium persulfate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106368027A true CN106368027A (en) | 2017-02-01 |
Family
ID=57891191
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611012126.6A Pending CN106368027A (en) | 2016-11-17 | 2016-11-17 | Method for preparing nanocellulose through oxidative degradation of ammonium persulfate |
Country Status (1)
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| CN (1) | CN106368027A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108221438A (en) * | 2017-12-07 | 2018-06-29 | 华南理工大学 | A kind of preparation method of bleached eucalyptus pulp nano-cellulose |
| CN114016149A (en) * | 2021-08-31 | 2022-02-08 | 南京森奇新材料科技有限公司 | Cellulose fiber, cellulose fiber dispersion liquid and preparation method thereof |
-
2016
- 2016-11-17 CN CN201611012126.6A patent/CN106368027A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108221438A (en) * | 2017-12-07 | 2018-06-29 | 华南理工大学 | A kind of preparation method of bleached eucalyptus pulp nano-cellulose |
| CN114016149A (en) * | 2021-08-31 | 2022-02-08 | 南京森奇新材料科技有限公司 | Cellulose fiber, cellulose fiber dispersion liquid and preparation method thereof |
| CN114016149B (en) * | 2021-08-31 | 2023-11-28 | 南京森奇新材料科技有限公司 | Cellulose fiber, cellulose fiber dispersion liquid and preparation method thereof |
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| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170201 |
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| WD01 | Invention patent application deemed withdrawn after publication |