CN106638088A - Method for preparing nano cellulose by utilizing neutral sulfite pretreatment plant fibers - Google Patents
Method for preparing nano cellulose by utilizing neutral sulfite pretreatment plant fibers Download PDFInfo
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- CN106638088A CN106638088A CN201611039854.6A CN201611039854A CN106638088A CN 106638088 A CN106638088 A CN 106638088A CN 201611039854 A CN201611039854 A CN 201611039854A CN 106638088 A CN106638088 A CN 106638088A
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- cellulose
- neutral sulfite
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- plant fibers
- string
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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
- D21C3/00—Pulping cellulose-containing materials
- D21C3/04—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides
- D21C3/06—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides sulfur dioxide; sulfurous acid; bisulfites sulfites
-
- 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
- D21C3/06—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides sulfur dioxide; sulfurous acid; bisulfites sulfites
- D21C3/08—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides sulfur dioxide; sulfurous acid; bisulfites sulfites calcium bisulfite
-
- 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
- D21C3/06—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides sulfur dioxide; sulfurous acid; bisulfites sulfites
- D21C3/10—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides sulfur dioxide; sulfurous acid; bisulfites sulfites magnesium bisulfite
-
- 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
- D21C3/06—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides sulfur dioxide; sulfurous acid; bisulfites sulfites
- D21C3/12—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides sulfur dioxide; sulfurous acid; bisulfites sulfites sodium bisulfite
-
- 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
- D21C3/06—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides sulfur dioxide; sulfurous acid; bisulfites sulfites
- D21C3/14—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides sulfur dioxide; sulfurous acid; bisulfites sulfites ammonium bisulfite
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
- D21H11/12—Pulp from non-woody plants or crops, e.g. cotton, flax, straw, bagasse
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- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a method for preparing nano cellulose by utilizing plant fibers pretreated by neutral sulfite. The method comprises the following steps: pre-treating the crushed plant fibers with a neutral bisulfite solution, reserving the plant fibers via solid-liquid separation, washing and removing degradation products of the plant fibers in the pretreatment process; performing oxidation treatment on the plant fibers with an oxidation system, then repeatedly centrifuging and washing to obtain oxidized plant fibers; performing cyclic homogenate treatment and ultrasonic treatment on the oxidized plant fibers, centrifuging and collecting an supernatant, namely nano fiber dispersion liquid; performing freezing and drying treatment on the nano fiber dispersion liquid to obtain the nano cellulose. The method disclosed by the invention has the benefits that the nano cellulose is prepared by utilizing the plant fibers pretreated by the neutral sulfite, raw materials are not required to remove hemi-cellulose and lignin step by step, the production process is simple, the cost is low, the environment is protected, the cellulose purity of the pretreated plant fibers is high, and the prepared nano cellulose is high in stability and modulus; therefore, the industrial application prospect is huger.
Description
Technical field
The present invention relates to a kind of preparation method of nano-cellulose, and in particular to a kind of to be pre-processed using neutral sulfite
The method that string prepares nano-cellulose.
Background technology
The super-micro-fine fibres that nano-cellulose is diameter less than 100nm, with high-purity, high-cleanness, high, high Young's modulus,
The characteristics such as high intensity, and the lightweight with biomaterial, degradable, bio-compatible and the characteristic such as renewable, thus medical science,
There is huge application prospect in the fields such as electronic product, papermaking, building, automobile, food, cosmetics.
At present, nano-cellulose is mainly obtained by plant material, is primarily due to content of cellulose in plant material rich
Rich (accounting for 30%-50%), and cheap, abundance.Patent CN104651964A has invented a kind of cellulose Nanowire
The preparation method of dimension, with wood fiber biomass as raw material, after preimpregnation, the pretreatment of Jing steam blastings.Pretreated feedstock Jing again
High-temperature water heat treatment to be removed and wash suction filtration after hemicellulose, obtains hemicellulose hydrolysate and the filter rich in cellulose and lignin
Slag.Filter residue is in autoclave, plus ethylene glycol extraction lignin.Reaction terminates separation of solid and liquid, obtains lignin extract and fibre
The plain solid of dimension, cellulose solids Jing cellulase degradation removes amorphous region and obtains cellulose crystals, and cellulose crystals are high-pressure homogeneous
Nano-cellulose finished product is obtained afterwards.The method is loaded down with trivial details to the pretreating process of fibrous raw material and energy consumption is higher；Patent
CN104762846A has invented a kind of preparation method of cotton stalk bark fiber element nano whisker, adopts cotton stalk skins for raw material, and Jing locates in advance
After reason, biochemical treatment, carry out mechanical crushing and obtain cotton stalk bark fiber element powder；Again Jing DMSO are processed and TEMPO oxidation processes, high
The cotton stalk bark fiber element powder suspension that speed stirring is obtained.Then centrifugal treating, decentralized processing and freeze-drying are carried out again, are obtained
Cotton stalk bark fiber element nano whisker.The biochemical treatment of the method needs to add enzyme, increased cost, is not suitable for large-scale production.
Sulphite pretreatment of fiber raw material can suitably reduce xylan, and pre- place while effectively removing lignin
Accessory substance is produced during reason few, therefore the fibrous raw material of this kind of pretreatment prepares nano-cellulose and will greatly simplify technique mistake
Journey, is more suitable for industrialized production.
The content of the invention
The technical problem to be solved is to provide a kind of using the preparation of neutral sulfite preprocessing plant fibre
The method of nano-cellulose, simplifies production technology, reduces production cost, improves industrial applications prospect.
To solve above-mentioned technical problem, the technical solution adopted in the present invention is as follows：
A kind of method that utilization neutral sulfite preprocessing plant fibre prepares nano-cellulose, the method includes as follows
Step：
1) by the string crushed Jing after the pretreatment of neutral sulfite hydrogen salt solution, separation of solid and liquid retains string,
Washing removes the catabolite of string in preprocessing process；
2) by step 1) after the oxidized system oxidation processes of string that obtain, it is centrifuged repeatedly, cleaning obtains oxidation and plants
Fibres；
3) by step 2) the oxidation string that obtains circulation homogenized, it is ultrasonically treated after, supernatant is collected by centrifugation and is
Nanofiber dispersion liquid；
4) by step 3) the nanofiber dispersion liquid freeze-drying process that obtains obtains final product nano-cellulose.
Step 1) in, described string is maize straw, wheat stalk, paddy rice stalk stalk, bagasse and alfa
In one or more of mixture；It is crushed to 20-80 mesh, preferably 80 mesh.
Step 1) in, described neutral sulfite hydrogen salt solution is the bisulfite solution of pH 5.0-8.0, described
Bisulfites be magnesium bisulfite, sodium hydrogensulfite, ammonium bisulfite or calcium bisulfite, preferred magnesium bisulfite；It is described
Neutral sulfite hydrogen salt solution compound method be：Bisulfite salinity be 4-8wt% (preferred 6wt%), sulphite with
The ratio of acid is 1g: (2-6) (preferred 1g: 4mL), remaining solvent is water to mL, and described acid is sulfuric acid or sulfurous acid, preferred sulfurous
Acid.
Step 1) in, described string and described neutral sulfite hydrogen salt solution solid-to-liquid ratio is 1g: (4-8) mL,
It is preferred that 1g: 6mL；Described preprocess method is：In sealed reactor, using neutral sulfite hydrogen salt solution and string
It is sufficiently mixed, temperature programming to 140-170 DEG C (preferably 170 DEG C) is reacted afterwards after 10-60min (preferred 60min), cools down, discharging.
Step 2) in, described oxidation system is non-selective oxidation and selective oxidation；Described non-selective oxidation
System is any one in sodium hypochlorite, hydrogen peroxide or persulfuric acid, preferred sodium hypochlorite；Selective oxidation system was iodine
Acid, periodates, NO2、N2O4, the phosphoric acid solution of natrium nitrosum, the phosphoric acid solution of sodium nitrate, sodium bromate, sodium chlorate, chlorous acid
Any one in sodium, hypochlorite, TEMPO, preferred TEMPO.
Step 2) in, the temperature of oxidation processes is 0-30 DEG C, and preferably 25 DEG C, the time is 1-3h, preferred 2h.
Step 2) in, described centrifugation is 5000-10000rpm, preferred 8000rpm, 5-10min, and preferred 6min is stayed
Water-insoluble.
Step 3) in, by step 2) the oxidation string homogenized that obtains is：By 0.1-1g (preferred 0.1g) over dry
The step of 2) the oxidation string that obtains, in being added to 100-1000mL (preferred 100mL) distilled water, refiner is homogenized
Process 10-60s (preferred 30s)；Described is ultrasonically treated for ultrasonically treated 1-5min (preferred 3min)；Circulate homogenized and surpass
Sonication 3-10 time (preferably 6 times).
Step 3) in, described centrifugation is that 8000-10000rpm (preferred 10000rpm) centrifugation 3-10min are (preferred
6min)。
Step 4) in, freeze-drying temperature is -40 DEG C -- 60 DEG C, preferably -50 DEG C.
The present invention is used for neutral sulfite pretreatment of fiber raw material to prepare nano-cellulose, and simplification prepares nanofiber
The process route of element, reduces production cost, obtains the nano-cellulose of high stability, modulus, is the production of nano-cellulose
And prepare with scale provides new approaches and new technology.Raw material removes hemicellulose and lignin, production technology letter without the need for substep
List, low cost, environmental friendliness, preprocessing plant fibre cellulose purity is high, the nano-cellulose stability of preparation, modulus height,
With more huge prospects for commercial application.
The present invention has the advantage that compared with the nano-cellulose preparation of document report or production technology：
1. sulphite pretreatment of fiber raw material can simultaneously remove hemicellulose and lignin.
2. technique is simpler, more convenient to operate.
3. the sulphite pretreatment of fiber raw cellulose purity for obtaining is high.
4., with agriculture and forestry organic waste materials such as stalk, alfas as raw material, production cost is reduced.
5. nano-cellulose heat endurance height, the modulus height for preparing, increased the prospects for commercial application of nano-cellulose.
Description of the drawings
Fig. 1 is the schematic diagram of the technical process of the present invention.
Fig. 2 is the transmission electron microscope picture of the nano-cellulose of the present invention.
Fig. 3 is the atomic force microscopy diagram of the nano-cellulose of the present invention.
Fig. 4 is the thermogravimetric analysis figure of the nano-cellulose of the present invention.
Specific embodiment
Below in conjunction with Application Example, the invention will be further elaborated.Embodiment is sent out for illustrative and not limiting
It is bright.Any those of ordinary skill in this area can be done suitable it will be appreciated that these embodiments limit never in any form the present invention
When modification and without prejudice to the present invention essence and deviate the scope of the present invention.
Embodiment 1
80 mesh are screened after using small plant pulverizer is crushed wheat stalk.Weighing 50g over dry straws, to be placed in 1L closed
In reactor, according to solid-to-liquid ratio 1g：6mL adds pretreatment fluid.Described pretreatment fluid includes 6wt% magnesium bisulfites, wherein
Magnesium bisulfite: sulfurous acid consumption=1g: 4mL, solvent is water.Capping kettle, in being placed in oil bath reactor.Oil bath reactor
170 DEG C are warming up to from 30 DEG C with 1 DEG C/min, along with mixing, rotating speed 10rpm in temperature-rise period.It is warming up to 170 DEG C of guarantors
After warm 60min, taking-up reactor is immediately placed in cold water and is cooled to after room temperature, discharging, separation of solid and liquid, pretreated material distillation
Water washing is dried to neutrality.The composition such as table 1 of wheat stalk, content of cellulose 73.43wt%, half fiber after analysis pretreatment
Element and lignin are respectively 9.52wt% and 10.40wt%.
Straw constituent analysis table after pre-processing in the embodiment 1 of table 1
Embodiment 2
Weigh 25 DEG C of the over dry wheat stalk Jing TEMPO selective oxidations system obtained after a certain amount of embodiment 1 is processed
After oxidation 2h, mixed liquor is centrifuged 6min under 8000rpm, outwells supernatant, adds and continues centrifugally operated after distilled water, repeats 6
More than secondary.Water-insoluble is left for selective oxidation cellulose.
Embodiment 3
Weigh the over dry wheat stalk Jing sodium hypochlorite non-selective oxidation systems obtained after a certain amount of embodiment 1 is processed
After 25 DEG C of oxidation 2h, mixed liquor is centrifuged 6min under 8000rpm, outwells supernatant, to add and continue centrifugally operated after distilled water, weight
It is multiple more than 6 times.Water-insoluble is left for non-selective oxidation cellulose.
Embodiment 4
Weigh 0.1g dry weight oxycelluloses (oxycellulose that embodiment 2 or 3 is obtained) to add in 100mL distilled water,
Ultrasonically treated 3min after homogenized 30s, circulation homogenate ultrasound six times are carried out using refiner.With the centrifugation of 10000rpm rotating speeds
6min, collects supernatant, as cellulose nano-fibrous dispersion liquid.Analyze its mechanical property as shown in table 2, obtaining Young's modulus is
5684.32Mpa, stress is 140.91Mpa, is strained as 5.37%.By transmission electron microscope (such as Fig. 2) and AFM (such as
Fig. 3) analyze its microscopic appearance feature, it is possible to find obvious nano-cellulose, average length is 50-100nm, and mean breadth is
10-20nm.- 50 DEG C of freeze-drying process of nano dispersion fluid are obtained into nano-cellulose powder, thermogravimetric analysis (such as Fig. 4) understands it most
Whole rate of weight loss is significantly lower than raw material, and heat endurance is high.
The mechanical property parameters statistical form of nano-cellulose obtained in the embodiment 4 of table 2
Claims (10)
1. a kind of method that utilization neutral sulfite preprocessing plant fibre prepares nano-cellulose, it is characterised in that the party
Method comprises the steps：
1) by the string crushed Jing after the pretreatment of neutral sulfite hydrogen salt solution, separation of solid and liquid retains string, washing
Remove the catabolite of string in preprocessing process；
2) by step 1) after the oxidized system oxidation processes of string that obtain, it is centrifuged repeatedly, cleaning obtains aoxidizing plant fine
Dimension；
3) by step 2) the oxidation string that obtains circulation homogenized, it is ultrasonically treated after, supernatant is collected by centrifugation and is nanometer
Fiber dispersion；
4) by step 3) the nanofiber dispersion liquid freeze-drying process that obtains obtains final product nano-cellulose.
2. utilization neutral sulfite solution preprocessing plant fibre according to claim 1 prepares the side of nano-cellulose
Method, it is characterised in that step 1) in, described string be maize straw, wheat stalk, paddy rice stalk stalk, bagasse and
The mixture of one or more in alfa；It is crushed to 20-80 mesh.
3. the method that utilization neutral sulfite preprocessing plant fibre according to claim 1 prepares nano-cellulose,
Characterized in that, step 1) in, described neutral sulfite hydrogen salt solution is the bisulfite solution of pH 5.0-8.0, described
Bisulfites be magnesium bisulfite, sodium hydrogensulfite, ammonium bisulfite or calcium bisulfite；Described neutral sulfite hydrogen
Salting liquid compound method is：Bisulfite salinity is 4-8wt%, and sulphite is 1g: (2-6) mL with the ratio of acid, remaining
Solvent is water, and described acid is sulfuric acid or sulfurous acid.
4. the method that utilization neutral sulfite preprocessing plant fibre according to claim 1 prepares nano-cellulose,
Characterized in that, step 1) in, described string is 1g with described neutral sulfite hydrogen salt solution solid-to-liquid ratio: (4-8)
mL；Described preprocess method is：In sealed reactor, fully mixed using neutral sulfite hydrogen salt solution and string
Close, temperature programming is reacted after 10-60min to after 140-170 DEG C, cool down, discharging.
5. the method that utilization neutral sulfite preprocessing plant fibre according to claim 1 prepares nano-cellulose,
Characterized in that, step 2) in, described oxidation system is non-selective oxidation and selective oxidation；Described non-selective oxygen
Change system is any one in sodium hypochlorite, hydrogen peroxide or persulfuric acid；Selective oxidation system is periodic acid, periodic acid
Salt, NO2、N2O4, the phosphoric acid solution of natrium nitrosum, the phosphoric acid solution of sodium nitrate, sodium bromate, sodium chlorate, sodium chlorite, hypochlorous acid
Any one in salt, TEMPO.
6. the method that utilization neutral sulfite preprocessing plant fibre according to claim 1 prepares nano-cellulose,
Characterized in that, step 2) in, the temperature of oxidation processes is 0-30 DEG C, and the time is 1-3h.
7. the method that utilization neutral sulfite preprocessing plant fibre according to claim 1 prepares nano-cellulose,
Characterized in that, step 2) in, described centrifugation is 5000-10000rpm, 5-10min, leaves water-insoluble.
8. the method that utilization neutral sulfite preprocessing plant fibre according to claim 1 prepares nano-cellulose,
Characterized in that, step 3) in, by step 2) the oxidation string homogenized that obtains is：By the step of 0.1-1g over dry 2)
The oxidation string for obtaining, in being added to 100-1000mL distilled water, refiner carries out homogenized 10-60s；Described is super
Sonication is ultrasonically treated 1-5min；Circulation homogenized and ultrasonically treated 3-10 time.
9. the method that utilization neutral sulfite preprocessing plant fibre according to claim 1 prepares nano-cellulose,
Characterized in that, step 3) in, described centrifugation is that 8000-10000rpm is centrifuged 3-10min.
10. the method that utilization neutral sulfite preprocessing plant fibre according to claim 1 prepares nano-cellulose,
Characterized in that, step 4) in, freeze-drying temperature is -40 DEG C -- 60 DEG C.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107201685A (en) * | 2017-05-17 | 2017-09-26 | 武汉理工大学 | The pilot production line and its technique of Cellulose nanocrystal are extracted from biomass resource |
| CN108641146A (en) * | 2018-04-04 | 2018-10-12 | 史国民 | A kind of oil resistant rubber sealing member material and preparation method thereof |
| CN109250990A (en) * | 2018-11-17 | 2019-01-22 | 长沙浩然医疗科技有限公司 | A kind of production technology of environmental protection furniture material |
| CN109485736A (en) * | 2018-12-05 | 2019-03-19 | 昆明理工大学 | A method of preparing nanocrystal cellulose |
| CN112480182A (en) * | 2020-12-22 | 2021-03-12 | 南京林业大学 | Preparation method of low-molecular-weight lignin and application of low-molecular-weight lignin in preparation of monophenol compounds |
| CN116943840A (en) * | 2023-08-07 | 2023-10-27 | 广州绿徽新材料研究院有限公司 | Device for high-speed three-vortex-microwave composite super-nano grinding of plant fiber powder by pressure change cavitation |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107201685A (en) * | 2017-05-17 | 2017-09-26 | 武汉理工大学 | The pilot production line and its technique of Cellulose nanocrystal are extracted from biomass resource |
| CN107201685B (en) * | 2017-05-17 | 2019-01-22 | 武汉理工大学 | The pilot production line and its technique of Cellulose nanocrystal are extracted from biomass resource |
| CN108641146A (en) * | 2018-04-04 | 2018-10-12 | 史国民 | A kind of oil resistant rubber sealing member material and preparation method thereof |
| CN108641146B (en) * | 2018-04-04 | 2020-11-27 | 苏州鱼得水电气科技有限公司 | Oil-resistant rubber sealing element material and preparation method thereof |
| CN112409660A (en) * | 2018-04-04 | 2021-02-26 | 史国民 | Oil-resistant rubber sealing element material |
| CN112409660B (en) * | 2018-04-04 | 2023-04-25 | 宏阳鑫精密科技(福建)有限公司 | Oil-resistant rubber sealing element material |
| CN109250990A (en) * | 2018-11-17 | 2019-01-22 | 长沙浩然医疗科技有限公司 | A kind of production technology of environmental protection furniture material |
| CN109485736A (en) * | 2018-12-05 | 2019-03-19 | 昆明理工大学 | A method of preparing nanocrystal cellulose |
| CN112480182A (en) * | 2020-12-22 | 2021-03-12 | 南京林业大学 | Preparation method of low-molecular-weight lignin and application of low-molecular-weight lignin in preparation of monophenol compounds |
| CN116943840A (en) * | 2023-08-07 | 2023-10-27 | 广州绿徽新材料研究院有限公司 | Device for high-speed three-vortex-microwave composite super-nano grinding of plant fiber powder by pressure change cavitation |
| CN116943840B (en) * | 2023-08-07 | 2024-04-09 | 广州绿徽新材料研究院有限公司 | Device for high-speed three-vortex-microwave composite super-nano grinding of plant fiber powder by pressure change cavitation |
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