CN106381744A - Method for separating nano cellulose from reeds - Google Patents
Method for separating nano cellulose from reeds Download PDFInfo
- Publication number
- CN106381744A CN106381744A CN201610962761.4A CN201610962761A CN106381744A CN 106381744 A CN106381744 A CN 106381744A CN 201610962761 A CN201610962761 A CN 201610962761A CN 106381744 A CN106381744 A CN 106381744A
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- CN
- China
- Prior art keywords
- cellulose
- nano
- solution
- reeds
- phragmites communiss
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Classifications
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- 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
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/10—Bleaching ; Apparatus therefor
- D21C9/16—Bleaching ; Apparatus therefor with per compounds
- D21C9/163—Bleaching ; Apparatus therefor with per compounds with peroxides
-
- 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
- D21C3/04—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides
-
- 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
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/02—Washing ; Displacing cooking or pulp-treating liquors contained in the pulp by fluids, e.g. wash water or other pulp-treating agents
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a method for separating nano cellulose from reeds. The method comprises the following steps: drying reeds at 80 DEG C to constant weight, pulverizing and screening; carrying out stirring hydrolysis on the cellulose raw material by using a sodium hydroxide solution; filtering the hydrolyzed precipitate, and bleaching with a bleacher to obtain cellulose; carrying out freeze-drying on the cellulose, and carrying out degradation and separation by using sulfuric acid to obtain nano cellulose; and centrifugating and cleaning for later use. The reeds in the natural world used as the raw material have the advantages of wide distribution, high growth speed and the like. Schistosomes can easily produce in the reeds, so that the method changes wastes into valuable substances; and the reeds used as the raw material can inhibit the breeding of insects. The method is efficient and sustainable. The sodium hydroxide hydrolysis can reduce the consumption of sulfuric acid in the later period; and the obtained nano cellulose has a certain dimensional range, and can be used in the fields of nano medicine, nano food and the like.
Description
Technical field
The invention belongs to natural macromolecular material field, a kind of particularly method preparing nano-cellulose.
Background technology
Cellulose is the natural macromolecular material that in nature, plant is synthesized by photosynthesis, has and inexhaustible uses it
Inexhaustible advantage.Nano-cellulose compared with native cellulose, have high-purity, high polymerization degree, high-crystallinity, high-hydrophilic,
The research of the advantages of high Young's modulus, high transparent, therefore its preparation and application is international emphasis and focus.Preparation is received at present
The method of rice cellulose is more, and such as Mechanical Method, chemical method, bioanalysises have all successfully prepared the material of excellent performance, but at present
Shortcoming focuses primarily upon chemical reagent cost, energy expenditure, and the requirement of time length and equipment, therefore, at present to nano-cellulose
Prepare Main way be developing low-cost and efficient technology.
The present invention proposes a kind of method separating nano-cellulose from phragmites communiss, by the use of the phragmites communiss in nature as former
Material, have widely distributed, growth quick the advantages of.It is also the place that schistosomicide is easily grown in phragmites communiss, turn waste into wealth and utilize reed
Reed can suppress the procreation of insects as raw material.Method used by the present invention has high efficiency and sustainability, the hydrogen-oxygen of early stage
Change the consumption that sodium hydrolysis can reduce later stage sulphuric acid, obtain nano-cellulose and there is certain size range, can cure as nanometer
The fields such as medicine, nanometer food.
Content of the invention
For overcoming the deficiencies in the prior art, the present invention provides a kind of method separating nano-cellulose from phragmites communiss, the party
Method has high efficiency and sustainability, by the use of the phragmites communiss in nature as raw material, can turn waste into wealth, and can suppress insects again
Procreation.
The object of the invention is realized by following proposal：
A kind of from phragmites communiss separate nano-cellulose method it is characterised in that：Phragmites communiss are first dried to constant weight under the conditions of 80 DEG C
After pulverize and sieve, sodium hydroxide solution cellulosic material is stirred hydrolyze, the precipitate after hydrolysis after filtering with bleaching
Agent carries out bleaching and obtains cellulose, and cellulose is freeze-dried, and then sulphuric acid degraded separates and obtains nano-cellulose, eccentric cleaning
Stand-by.
The mass concentration of the sodium hydroxide of described hydrolysis material is 15 ~ 30%；Raw material with the solid-to-liquid ratio of sodium hydroxide solution is
1:(10~20)；The condition of hydrolysis is 90 ~ 170 DEG C of reaction 3 ~ 10h；Solution stirring speed is 500 ~ 2000rpm.
Granular size after sieving is 20 mesh sieves to 40 mesh sieves, and mean diameter is 0.83 ~ 0.38mm.
It is dissolved in deionized water after the solution bleached filters after described hydrolysis, filtrate again:Deionized water=1:3, use
Acid for adjusting pH=7；Add bleach.
Described addition bleach is one kind of hydrogen peroxide or sodium hypochlorite, and mass concentration is（20~40%）；Bleaching temperature
50 ~ 90 DEG C, the time is 3 ~ 10h.
Reactant after described bleaching is cellulose mixed liquor, then carries out lyophilization, and dried pure cellulose is used
Sulphuric acid carries out degraded and separates, and h 2 so 4 concentration is 50 ~ 80%, and cellulose is 1 with the mass ratio of sulfuric acid solution:25, the time be 1 ~
4 hours, obtain nano-cellulose solution.
The washing of described nano-cellulose solution centrifugal, the speed of centrifugation is 10000 ~ 15000rmp, centrifugation time 5 ~
15min, forms white gels, and the nano-cellulose gel solution that quality is 1% made by sample.
It is an advantage of the current invention that：Nano-cellulose raw material of the present invention has a sustainability, being suitable for of early stage sodium hydroxide
The consumption of sulphuric acid can be reduced, can obtain additionally by the degradation time controlling later stage sulfuric acid solution and there is various sizes of receiving
Rice cellulose, has simple to operate, the advantages of being easily controlled.The method has high efficiency and sustainability, using in nature
Phragmites communiss as raw material, can turn waste into wealth, the procreation of insects can be suppressed again.
Phragmites communiss in nature, as raw material, have widely distributed, growth quick the advantages of.It is also that schistosomicide is held in phragmites communiss
The place easily growing, is turned waste into wealth and can be suppressed the procreation of insects by the use of phragmites communiss as raw material.The present invention is had using method
High efficiency and sustainability, first can reduce the consumption of later stage sulphuric acid with sodium hydroxide hydrolysis, obtain nano-cellulose and have necessarily
Size range, can be used as fields such as nanometer medicine, nanometer foods.
Brief description
Fig. 1 is the nano-cellulose SEM figure of the embodiment of the present invention 1.
Specific embodiment
Embodiment 1：
Weigh phragmites communiss 50g, 80 DEG C are dried to constant weight in an oven, be then comminuted into granule, the size of granule is 20 mesh sieves to 40
Between mesh sieve, mean diameter is 0.567mm-5.06mm；The NaOH solution weighing 88g adds the deionized water of 412ml, prepares
The sodium hydroxide solution of 15wt%；React 10h at 170 DEG C, the mixing speed of solution is 2000rpm；Deionized water with 3 times is clear
After washing, adjust pH=7;
Add the hydrogen peroxide of mass concentration 20% in the solution, partially white 3h, obtains cellulose mixed liquor at 50 DEG C；Freezing is dry
Obtain pure cellulose after dry, prepare the sulfuric acid solution of 50wt%, the ratio of cellulose and sulphuric acid is 1:25, degrade 1 hour, received
Rice cellulose, size is about 260nm, as shown in Figure 1；10000rpm is centrifuged 5min, obtains white gels, is configured to 1% solution
Stand-by.
Embodiment 2：
Weigh phragmites communiss 50g, 80 DEG C are dried to constant weight in an oven, be then comminuted into granule, the size of granule is 20 mesh sieves to 40
Between mesh sieve, mean diameter is 0.567mm-5.06mm；The NaOH solution weighing 300g adds the deionized water of 700ml, prepares
The sodium hydroxide solution of 30wt%；React 10h at 90 DEG C, the mixing speed of solution is 500rpm；Cleaned with 3 times of deionized water
Afterwards, adjust pH=7;Add the hydrogen peroxide of mass concentration 40% in the solution, partially white 10h, obtains cellulose mixing at 90 DEG C
Liquid；Obtain pure cellulose after lyophilization, prepare the sulfuric acid solution of 80wt%, the ratio of cellulose and sulphuric acid is 1:25, degraded 4 is little
When, obtain nano-cellulose, size is about 180nm；15000rpm is centrifuged 15min, obtains white gels, is configured to 1% solution
Stand-by.
Embodiment 3：
Weigh phragmites communiss 50g, 80 DEG C are dried to constant weight in an oven, be then comminuted into granule, the size of granule is 20 mesh sieves to 40
Between mesh sieve, mean diameter is 0.567mm-5.06mm；The NaOH solution weighing 150g adds the deionized water of 350ml, prepares
The sodium hydroxide solution of 25wt%；React 6h at 120 DEG C, the mixing speed of solution is 1500rpm；Cleaned with 3 times of deionized water
Afterwards, adjust pH=7;Add the hydrogen peroxide of mass concentration 30% in the solution, partially white 10h, obtains cellulose mixing at 70 DEG C
Liquid；Obtain pure cellulose after lyophilization, prepare the sulfuric acid solution of 80wt%, the ratio of cellulose and sulphuric acid is 1:25, degraded 2.5
Hour, obtain nano-cellulose, size is about 210nm；12500rpm be centrifuged 10min, obtain white gels, be configured to 1% molten
Liquid is stand-by.
Embodiment 4：
Weigh phragmites communiss 50g, 80 DEG C are dried to constant weight in an oven, be then comminuted into granule, the size of granule is 20 mesh sieves to 40
Between mesh sieve, mean diameter is 0.567mm-5.06mm；The NaOH solution weighing 88g adds the deionized water of 412ml, prepares
The sodium hydroxide solution of 15wt%；React 10h at 170 DEG C, the mixing speed of solution is 2000rpm；Deionized water with 3 times is clear
After washing, adjust pH=7;
Add the sodium hypochlorite of mass concentration 20% in the solution, partially white 3h, obtains cellulose mixed liquor at 50 DEG C；Freezing is dry
Obtain pure cellulose after dry, prepare the sulfuric acid solution of 50wt%, the ratio of cellulose and sulphuric acid is 1:25, degrade 1 hour, received
Rice cellulose, size is about 250nm；10000rpm is centrifuged 5min, obtains white gels, is configured to 1% solution for later use.
Claims (7)
1. a kind of from phragmites communiss separate nano-cellulose method it is characterised in that：Phragmites communiss are first dried to perseverance under the conditions of 80 DEG C
Pulverize and sieve after weight, sodium hydroxide solution is stirred to cellulosic material hydrolyzing, the precipitate after hydrolysis is after filtering with drift
White agent carries out bleaching and obtains cellulose, and cellulose is freeze-dried, and then sulphuric acid degraded separates and obtains nano-cellulose, and centrifugation is clear
Wash stand-by.
2. as described in claim 1 a kind of from phragmites communiss separate nano-cellulose method it is characterised in that：Described hydrolysis material
Sodium hydroxide mass concentration be 15 ~ 30%；Raw material is 1 with the solid-to-liquid ratio of sodium hydroxide solution:(10~20)；Hydrolysis
Condition is 90 ~ 170 DEG C of reaction 3 ~ 10h；Solution stirring speed is 500 ~ 2000rpm.
3. as described in claim 1 a kind of from phragmites communiss separate nano-cellulose method it is characterised in that：Granule after sieving
Size is 20 mesh sieves to 40 mesh sieves, and mean diameter is 0.83 ~ 0.38mm.
4. as described in claim 1 a kind of from phragmites communiss separate nano-cellulose method it is characterised in that：After described hydrolysis
It is dissolved in deionized water after the solution bleached filters, filtrate again:Deionized water=1:3, using acid for adjusting pH=7；Add drift
White agent.
5. as described in claim 1 a kind of from phragmites communiss separate nano-cellulose method it is characterised in that：Described addition drift
White agent is one kind of hydrogen peroxide or sodium hypochlorite, and mass concentration is（20~40%）；50 ~ 90 DEG C of bleaching temperature, the time be 3 ~
10h.
6. as described in claim 1 a kind of from phragmites communiss separate nano-cellulose method it is characterised in that：After described bleaching
Reactant be cellulose mixed liquor, then carry out lyophilization, dried pure cellulose sulphuric acid carry out degraded separate, sulfur
Sour mass concentration is 50 ~ 80%, and cellulose is 1 with the mass ratio of sulfuric acid solution:25, the time is 1 ~ 4 hour, obtains nanofiber
Plain solution.
7. as described in claim 6 a kind of from phragmites communiss separate nano-cellulose method it is characterised in that：Described Nanowire
Dimension plain solution centrifugal washing, the speed of centrifugation is 10000 ~ 15000rmp, centrifugation time 5 ~ 15min, forms white gels, sample
Make the nano-cellulose gel solution that quality is 1%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610962761.4A CN106381744A (en) | 2016-10-28 | 2016-10-28 | Method for separating nano cellulose from reeds |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610962761.4A CN106381744A (en) | 2016-10-28 | 2016-10-28 | Method for separating nano cellulose from reeds |
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| CN106381744A true CN106381744A (en) | 2017-02-08 |
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ID=57957267
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610962761.4A Pending CN106381744A (en) | 2016-10-28 | 2016-10-28 | Method for separating nano cellulose from reeds |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106939443A (en) * | 2017-04-10 | 2017-07-11 | 湖南易生环保新材料有限公司 | A kind of reed stem cellulose nano wire and preparation method thereof |
| CN112220935A (en) * | 2020-09-23 | 2021-01-15 | 华南理工大学 | Camellia oleifera shell carboxyl fiber nano material and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011072365A1 (en) * | 2009-12-15 | 2011-06-23 | National Research Council Of Canada | Cellulose nanocrystals from renewable biomass |
| CN104387478A (en) * | 2014-12-17 | 2015-03-04 | 菏泽市产品质量监督检验所 | Preparation method of peony stem nano-cellulose for oil |
| CN104674586A (en) * | 2015-02-02 | 2015-06-03 | 天津市浩宇助剂有限公司 | Preparation process of nano cellulose whisker |
| CN104963228A (en) * | 2015-07-16 | 2015-10-07 | 吉林大学 | Method for preparing nano cellulose by utilizing sunflower seed husks |
| CN105568744A (en) * | 2015-12-17 | 2016-05-11 | 华南理工大学 | Cornstalk nanocellulose whiskers and preparation method and application thereof |
-
2016
- 2016-10-28 CN CN201610962761.4A patent/CN106381744A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011072365A1 (en) * | 2009-12-15 | 2011-06-23 | National Research Council Of Canada | Cellulose nanocrystals from renewable biomass |
| CN104387478A (en) * | 2014-12-17 | 2015-03-04 | 菏泽市产品质量监督检验所 | Preparation method of peony stem nano-cellulose for oil |
| CN104674586A (en) * | 2015-02-02 | 2015-06-03 | 天津市浩宇助剂有限公司 | Preparation process of nano cellulose whisker |
| CN104963228A (en) * | 2015-07-16 | 2015-10-07 | 吉林大学 | Method for preparing nano cellulose by utilizing sunflower seed husks |
| CN105568744A (en) * | 2015-12-17 | 2016-05-11 | 华南理工大学 | Cornstalk nanocellulose whiskers and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 刘潇等: "花生壳纳米纤维素的制备与表征", 《现代食品科技》 * |
| 谢成等: "碱处理芦苇浆纳米纤维素制备工艺条件优化", 《林产化学与工业》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106939443A (en) * | 2017-04-10 | 2017-07-11 | 湖南易生环保新材料有限公司 | A kind of reed stem cellulose nano wire and preparation method thereof |
| CN106939443B (en) * | 2017-04-10 | 2018-03-16 | 湖南工业大学 | A kind of reed stem cellulose nano wire and preparation method thereof |
| CN112220935A (en) * | 2020-09-23 | 2021-01-15 | 华南理工大学 | Camellia oleifera shell carboxyl fiber nano material and preparation method and application thereof |
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Application publication date: 20170208 |
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