CN104611967A - Reed pulp nano cellulose preparation method - Google Patents
Reed pulp nano cellulose preparation method Download PDFInfo
- Publication number
- CN104611967A CN104611967A CN201310537950.3A CN201310537950A CN104611967A CN 104611967 A CN104611967 A CN 104611967A CN 201310537950 A CN201310537950 A CN 201310537950A CN 104611967 A CN104611967 A CN 104611967A
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- Prior art keywords
- cellulose
- reed pulp
- microwave
- preparation
- nano
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- 235000014676 Phragmites communis Nutrition 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229920001046 Nanocellulose Polymers 0.000 title abstract 2
- 229920002678 cellulose Polymers 0.000 claims abstract description 41
- 239000001913 cellulose Substances 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000084 colloidal system Substances 0.000 claims abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000007062 hydrolysis Effects 0.000 claims abstract description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 235000010980 cellulose Nutrition 0.000 description 20
- 229920000168 Microcrystalline cellulose Polymers 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 235000019813 microcrystalline cellulose Nutrition 0.000 description 1
- 239000008108 microcrystalline cellulose Substances 0.000 description 1
- 229940016286 microcrystalline cellulose Drugs 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 235000001968 nicotinic acid Nutrition 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Paper (AREA)
Abstract
The invention relates to a reed pulp nano cellulose preparation method, reed pulp and 50-60% by mass of sulfuric acid are mixed in a reaction bottle, and stirred evenly, the mixture is put into a microwave reactor for pretreatment; the microwave temperature is 50 to 60 DEG C, the microwave time is 10-15min; suspension is obtained by hydrolysis for 4-5 hours at 50 to 60 DEG C; the suspension is centrifuged, and washed with deionized water until the pH value is 6-8; the ultrasonically treated product is centrifuged for 5-10min by use of an ultrasonic cell crusher, the ultrasonic power is 100W to obtain cellulose colloid; the cellulose colloid is into a drying box for drying at 40 to 50 DEG C until the weight is constant to obtain a reed pulp cellulose solid. The yield of the reed pulp cellulose prepared by the method is high, and the calculated yield can reach 55% in optimal reaction conditions, and the preparation method is simple, easy to duplicate, and suitable for industrial enlarged application.
Description
Technical field
The invention belongs to cellulose field, relate to nano-cellulose, particularly relate to a kind of preparation method of reed pulp nano-cellulose.
Background technology
Cellulose is that nature is synthesized by photosynthesis primarily of plant, inexhaustible, with it natural polymer without cease, be mainly used in the production departments such as weaving, papermaking, fine chemistry industry.Except traditional commercial Application, how to intersect and effectively utilize cellulose resource further in conjunction with subjects such as nano science, chemistry, physics, materialogy, biology and bionics, the application of developing cellulose in nanometer fine chemistry industry, nanometer medicine, nanometer food, nano composite material and new forms of energy, becomes the research topic that domestic and international scientist competitively carries out.
Handle cellulosic molecule and supramolecular aggregation thereof in nano-scale range, design and assemble stable multiple style, formulate out the new nanometer fine chemical product with excellent function, new nano material thus, become the Disciplinary Frontiers of Cellulose Science.Compared with powder cellulose and microcrystalline cellulose, nanofiber have many premium properties, as high-purity, high polymerization degree, high-crystallinity, high-hydrophilic, high Young's modulus, high strength, hyperfine structure and high transparent etc.Therefore, the research of the preparation of nano-cellulose, properity and application is being the emphasis studied of domestic and international cellulose chemistry and focus at present.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, a kind of preparation method of reed pulp nano-cellulose is provided.
The technical scheme that technical solution problem of the present invention adopts is:
A preparation method for reed pulp nano-cellulose, step is as follows:
(1) sulfuric acid being 50 ~ 60% by reed pulp and mass percentage mixes in reaction bulb, stirs;
(2) reaction bulb is put into microwave reactor preliminary treatment, microwave temperature 50 ~ 60 DEG C, microwave time 10 ~ 15min;
(3) by the reactant mixture through Microwave Pretreatment at 60 ~ 70 DEG C, be hydrolyzed 4 ~ 5 hours, obtain suspension;
(4) suspension is centrifugal, spending deionized water to pH value is 6 ~ 8;
(5) with Ultrasonic cell smash to the ultrasonic process 5 ~ 10min of the product after centrifugal treating, ultrasonic power 100W, obtains cellulose colloid;
(6) cellulose colloid is put into drying box, 40 ~ 50 DEG C are dried to constant weight, obtain reed pulp cellulose solids.
And microwave treatment temperature is 58 DEG C in described step (2).
And microwave treatment time is 13min in described step (2).
And hydrolysis temperature is 65 DEG C in described step (3).
And hydrolysis time is 4.5h in described step (3).
Advantage of the present invention and good effect are:
Reed pulp cellulose yield prepared by the present invention is high, and under the reaction condition of optimum, yield can reach 55% as calculated.And this preparation method is simple, easily repeats, is applicable to industry and amplifies application.
Detailed description of the invention:
Below in conjunction with accompanying drawing, also by specific embodiment, the invention will be further described, and following examples are descriptive, are not determinate, can not limit protection scope of the present invention with this.
Embodiment 1:
A preparation method for reed pulp nano-cellulose, step is as follows:
(1) sulfuric acid being 50 ~ 60% by reed pulp and mass percentage mixes in reaction bulb, stirs;
(2) reaction bulb is put into microwave reactor preliminary treatment, microwave temperature 50 DEG C, microwave time 10min;
(3) by the reactant mixture through Microwave Pretreatment at 60 DEG C, be hydrolyzed 4 hours, obtain suspension;
(4) suspension is centrifugal, spending deionized water to pH value is 6 ~ 8;
(5) with Ultrasonic cell smash to the ultrasonic process 5 ~ 10min of the product after centrifugal treating, ultrasonic power 100W, obtains cellulose colloid;
(6) cellulose colloid is put into drying box, 40 ~ 50 DEG C are dried to constant weight, obtain reed pulp cellulose solids.
Embodiment 2:
A preparation method for reed pulp nano-cellulose, step is as follows:
(1) sulfuric acid being 50 ~ 60% by reed pulp and mass percentage mixes in reaction bulb, stirs;
(2) reaction bulb is put into microwave reactor preliminary treatment, microwave temperature 60 DEG C, microwave time 15min;
(3) by the reactant mixture through Microwave Pretreatment at 70 DEG C, be hydrolyzed 5 hours, obtain suspension;
(4) suspension is centrifugal, spending deionized water to pH value is 6 ~ 8;
(5) with Ultrasonic cell smash to the ultrasonic process 5 ~ 10min of the product after centrifugal treating, ultrasonic power 100W, obtains cellulose colloid;
(6) cellulose colloid is put into drying box, 40 ~ 50 DEG C are dried to constant weight, obtain reed pulp cellulose solids.
Embodiment 3:
A preparation method for reed pulp nano-cellulose, step is as follows:
(1) sulfuric acid being 50 ~ 60% by reed pulp and mass percentage mixes in reaction bulb, stirs;
(2) reaction bulb is put into microwave reactor preliminary treatment, microwave temperature 58 DEG C, microwave time 13min;
(3) by the reactant mixture through Microwave Pretreatment at 65 DEG C, be hydrolyzed 4.5 hours, obtain suspension;
(4) suspension is centrifugal, spending deionized water to pH value is 6 ~ 8;
(5) with Ultrasonic cell smash to the ultrasonic process 5 ~ 10min of the product after centrifugal treating, ultrasonic power 100W, obtains cellulose colloid;
(6) cellulose colloid is put into drying box, 40 ~ 50 DEG C are dried to constant weight, obtain reed pulp cellulose solids.
Claims (5)
1. a preparation method for reed pulp nano-cellulose, is characterized in that: step is as follows:
(1) sulfuric acid being 50 ~ 60% by reed pulp and mass percentage mixes in reaction bulb, stirs;
(2) reaction bulb is put into microwave reactor preliminary treatment, microwave temperature 50 ~ 60 DEG C, microwave time 10 ~ 15min;
(3) by the reactant mixture through Microwave Pretreatment at 60 ~ 70 DEG C, be hydrolyzed 4 ~ 5 hours, obtain suspension;
(4) suspension is centrifugal, spending deionized water to pH value is 6 ~ 8;
(5) with Ultrasonic cell smash to the ultrasonic process 5 ~ 10min of the product after centrifugal treating, ultrasonic power 100W, obtains cellulose colloid;
(6) cellulose colloid is put into drying box, 40 ~ 50 DEG C are dried to constant weight, obtain reed pulp cellulose solids.
2. the preparation method of a kind of reed pulp nano-cellulose according to claim 1, is characterized in that: in described step (2), microwave treatment temperature is 58 DEG C.
3. the preparation method of a kind of reed pulp nano-cellulose according to claim 1, is characterized in that: in described step (2), microwave treatment time is 13min.
4. the preparation method of a kind of reed pulp nano-cellulose according to claim 1, is characterized in that: in described step (3), hydrolysis temperature is 65 DEG C.
5. the preparation method of a kind of reed pulp nano-cellulose according to claim 1, is characterized in that: in described step (3), hydrolysis time is 4.5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310537950.3A CN104611967A (en) | 2013-11-01 | 2013-11-01 | Reed pulp nano cellulose preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310537950.3A CN104611967A (en) | 2013-11-01 | 2013-11-01 | Reed pulp nano cellulose preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104611967A true CN104611967A (en) | 2015-05-13 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310537950.3A Pending CN104611967A (en) | 2013-11-01 | 2013-11-01 | Reed pulp nano cellulose preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104611967A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111019006A (en) * | 2019-12-13 | 2020-04-17 | 华南理工大学 | Method for preparing carboxylated nanocellulose by hydrolysis of citric acid under microwave condition |
| CN114075796A (en) * | 2020-08-20 | 2022-02-22 | 华南理工大学 | Plant-based cellulose nanofibrils as well as preparation method and application thereof |
| CN117720086A (en) * | 2024-02-07 | 2024-03-19 | 湖南裕能新能源电池材料股份有限公司 | Lithium iron manganese phosphate base material, positive electrode material, preparation method of positive electrode material and lithium battery |
-
2013
- 2013-11-01 CN CN201310537950.3A patent/CN104611967A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111019006A (en) * | 2019-12-13 | 2020-04-17 | 华南理工大学 | Method for preparing carboxylated nanocellulose by hydrolysis of citric acid under microwave condition |
| CN114075796A (en) * | 2020-08-20 | 2022-02-22 | 华南理工大学 | Plant-based cellulose nanofibrils as well as preparation method and application thereof |
| CN114075796B (en) * | 2020-08-20 | 2022-12-16 | 华南理工大学 | A plant-based cellulose nanofibril and its preparation method and application |
| CN117720086A (en) * | 2024-02-07 | 2024-03-19 | 湖南裕能新能源电池材料股份有限公司 | Lithium iron manganese phosphate base material, positive electrode material, preparation method of positive electrode material and lithium battery |
| CN117720086B (en) * | 2024-02-07 | 2024-05-14 | 湖南裕能新能源电池材料股份有限公司 | Lithium iron manganese phosphate substrate, positive electrode material and preparation method thereof, and lithium battery |
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| C06 | Publication | ||
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150513 |