CN104558210A - Method for preparing nano-cellulose - Google Patents
Method for preparing nano-cellulose Download PDFInfo
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Abstract
The invention belongs to the field of natural high-polymer materials, and particularly discloses a method for preparing nano-cellulose. The method comprises steps as follows: adding cellulose fibers and phosphotungstic acid powder to water, performing heating and stirring to obtain hydrocellulose fibers; adding an extracting agent to the obtained hydrocellulose fibers, collecting a supernatant and a subnatant respectively through extraction, and subjecting the supernatant to alcohol washing, water washing, centrifugation and freeze-drying processes to obtain nano-cellulose crystals; subjecting the subnatant to reduced-pressure distillation and recovery to collect the extracting agent and the phosphotungstic acid powder respectively for recycling. According to the method, the phosphotungstic acid which is good in hydrothermal stability, high in acidity, easy to recover and recyclable is used for replacing an inorganic liquid acid to hydrolyze the cellulose fibers to prepare the nano-cellulose; the method has the advantages that the method is simple to operate, safe and environment-friendly, and the prepared nano-cellulose is good in dispersibility and thermal stability.
Description
Technical field
The invention belongs to natural macromolecular material field, specifically a kind of method preparing nano-cellulose.
Background technology
Mierocrystalline cellulose is that occurring in nature distributes the widest and can carry out biodegradable natural polymer, is extensively present in the root of the plants such as trees, careless class, linen-cotton, stem and branches and leaves and some algea and bacteria.Mierocrystalline cellulose can be degraded by methods such as acid hydrolysis, enzymolysis, mechanical treatments and be obtained nano cellulose crystal.Nano-cellulose, as a kind of polymer-function material deriving from natural green renewable biomass, because it has excellent intensity and physical and chemical performance, has broad application prospects in fields such as biology, medicine, papermaking, food.
Traditional nano-cellulose preparation method mainly adopts mineral acid hydrolysis method, take cellulosic fibre as raw material, utilize the sulfuric acid that volumetric concentration is 45-60%, 2-24h is reacted at 0-38 DEG C, nanocrystal cellulose I powder is obtained through last handling processes such as washing, neutralizations, with obtaining nanocrystal cellulose II product (Chinese invention patent number: 01129717.4, title: the method for preparing nanocrystal cellulose by means of acid hydrolysis) after alkaline purification after neutralization is concentrated.The inorganic liquid acid corrosions such as the sulfuric acid that the method is used are strong, and high to equipment requirements, need add large water gaging stopped reaction, aftertreatment causes a large amount of spent acid solution, and environmental pollution is large.
Mierocrystalline cellulose is carried out pre-treatment by mechanical process, through high pressure shattering process, pressure is 1000-1200bar, and cycle index is 4-16 time, obtain nano-cellulose colloid (Chinese invention patent number: 201110151350.4, title: the broken subcooling of a kind of high pressure prepares the method for nano-cellulose).This method exists that energy consumption is large, cost is high, is not suitable for serialization and amplifies the shortcomings such as production.
Invention is had to use Biological preparation nano cellulose crystal, its main process is that paper pulp is immersed in 5%(w/w) aqueous sucrose solution in, after draining makes sugary paper pulp, mix with certain proportion with wheat bran, peptone, yeast, fermentation slurry (control temperature 30-35 DEG C is made in fermentor tank, fermentation time 70-75h), repeatedly grind by nano-level grinder and obtain nano-cellulose colloid (Chinese invention patent number: 201110002108.0, title: the bio-mechanical sub-wire method manufacturing nano-cellulose) for 5-15 time.This method efficiency is low, preparation process is complicated, require high to reaction environment.
Patent 200880117460.5 reports and adopts NaBr-TEMPO-NaClO oxidation system, natural cellulose micro-fibril C6 position primary hydroxyl group is oxidized, generating high density carboxyl sodium salt, obtained cellulose nano-fibrous (Chinese invention patent number: 200880117460.5, title: cellulose nano-fibrous and manufacture method, cellulose nano-fibrous dispersion liquid).Oxygenant TEMPO used by this method is poisonous, and it is many and without recovery process, be not suitable for amplifying production on a large scale that reaction process relates to chemical reagent.
Recent years, occur utilizing acidity/basic cation exchange resins hydrocellulose to prepare patent (Chinese invention patent number: 201010123123.6, the title: using basic anion-exchange resin prepares the method for nanocrystal cellulose II of nanocrystal cellulose; Chinese invention patent number: 201010123122.1, title: the method for nanocrystal cellulose I prepared by application acidic anionic exchange resin).This method overcomes the shortcoming of liquid acid/alkali really, but affects yield owing to can not carry out high efficiency separation to product, and Zeo-karb can not directly reuse, and needs regenerative process.
To sum up several method preparing nano-cellulose, mainly there is seriously polluted, the catalyzer problems such as recoverable or inefficiency, product yield be not high, so be badly in need of a kind of efficient, environmental protection and the nano-cellulose syntheti c route of the green of catalyzer reusable edible.
Summary of the invention
The object of the invention is the preparation method that a kind of nano cellulose crystal will be provided.
For achieving the above object, the technical solution used in the present invention is:
A kind of method preparing nano-cellulose:
1) phospho-wolframic acid hydrolysis fiber cellulose fiber: be added to the water by cellulose fiber peacekeeping phospho-wolframic acid powder, heated and stirred obtains hydrolysis fiber cellulose fiber;
2) be separated, purifying and recycle: in above-mentioned hydrocellulose fiber, add extraction agent, extraction collects the upper and lower liquid respectively, and upper liquid obtains nano cellulose crystal through alcohol wash, washing, centrifugal and freezing dry process; Subnatant underpressure distillation is reclaimed and is collected extraction agent and Powdered phospho-wolframic acid and then cycling and reutilization respectively.
Solid-liquid ratio is that the cellulosic fibre of 1:40-80 and phosphotungstic acid aqueous solution are added to the water by described step 1), at 50 DEG C-90 DEG C, stirs 15h-50h with the speed of 4000rpm-5000rpm; Wherein the mass concentration of phospho-wolframic acid in water is 50%-80%.
Described cellulosic fibre is one or both of wood pulps, Cotton Pulp, straw pulp or Microcrystalline Cellulose.
Described step 2) said hydrolyzed cellulosic fibre is mixed with the volume ratio of extraction agent according to 1:3-1:5, repeatedly extract 2-5 time, merge upper liquid and the subnatant of each time, upper liquid amasss 1-3 water washing doubly 3-5 time, then with the speed of 2000rpm-12000rpm with supernatant liquid again after upper liquid volume 1-3 alcohol alcohol wash 3-5 time doubly, alcohol wash; Centrifugal 3-5 time, each 10min-20min, obtains nano cellulose crystal finally by lyophilize; Subnatant 35 DEG C-45 DEG C, vacuum tightness be-0.5MPa ~ 0.1MPa under underpressure distillation reclaim and collect extraction agent and Powdered phospho-wolframic acid and then cycling and reutilization respectively.
Described catalyzer is ether.
The Powdered phospho-wolframic acid drying that described underpressure distillation is reclaimed is reusable edible afterwards.
Described alcohol can be one or more mixing in ethanol, methyl alcohol or butanols.
Principle illustrates, phospho-wolframic acid can dissociate H in aqueous as a kind of solid super strong heteropolyacid
+, there is B acid activity, remove the pars amorpha in Mierocrystalline cellulose grape sugar chain by hydrolysis reaction, prepare nano cellulose crystal.Meanwhile, phospho-wolframic acid can be separated with nano-cellulose by extracted with diethyl ether, by underpressure distillation, and phospho-wolframic acid and the equal reusable edible of ether.
The invention has the advantages that:
1. the phosphate-tungstic acid used in preparation process of the present invention is to environment toxicological harmless, and stable in properties, be easy to reclaim, reusable edible, meets the requirement of green Sustainable Production.
2. preparation process mild condition easy control of reaction system in the present invention, little to equipment corrosion, simple to operate.
3., compared with the present invention is hydrolyzed with conventional inorganic liquid acid, without a large amount of waste liquid output, water consumption is little.
4. simple to operate, the safety and environmental protection of preparation method of the present invention, catalyzer reusable edible, compared with the nano-cellulose prepared with traditional sulfuric acid process, rhabdolith nano-cellulose obtained by phospho-wolframic acid hydrolysis method of the present invention has very high Heat stability is good, is conducive to the application in matrix material enhancing body.
Accompanying drawing explanation
The process flow sheet that Fig. 1 provides for the embodiment of the present invention.
The phospho-wolframic acid hydrolysis wood pulps that Fig. 2 provides for the embodiment of the present invention prepares the transmission electron microscope picture of clubbed nano-cellulose.
Nano-cellulose (NCC) prepared by the paper pulp that Fig. 3 provides for the embodiment of the present invention, the present invention and sulfuric acid process prepare the thermal gravimetric analysis curve of nano-cellulose (s-NCC).
Fig. 4 prepares the transmission electron microscope picture of clubbed nano-cellulose for phospho-wolframic acid hydrolyzing microcrystalline cellulose that the embodiment of the present invention provides.
The phospho-wolframic acid hydrolysis wood pulps of the recycling that Fig. 5 provides for the embodiment of the present invention prepares the transmission electron microscope picture of clubbed nano-cellulose.
Specific examples mode
The present invention is illustrated by the following examples, but the present invention is not limited to following examples.
Embodiment 1
By Fig. 1, take 0.5g wood pulps and be placed in round-bottomed flask, add 40ml75% (w/w) phosphotungstic acid aqueous solution, at 90 DEG C, stir 30h with the speed mechanical of 4000rpm.After having reacted, rapid ice bath is to room temperature, with reaction solution: ether is that the volume ratio of 1:3 adds ether, extracting twice, lower floor's phospho-wolframic acid ether extraction liquid reclaims, and through 35 DEG C, vacuum tightness isolates phospho-wolframic acid solid for-0.5MPa rotary evaporation, ether reclaims through condensing works, phospho-wolframic acid and the equal reusable edible of ether; The ethanol of 3 times of volumes is added in the nanofiber cellulose solution of upper strata, be stirred to glass stick and mix, with the centrifugal 10min of the rotating speed of 6000rpm, throw out is poured out after centrifugal end, the ethanol adding 3 times of volumes in throw out mixes, with the centrifugal 10min of the rotating speed of 6000rpm, after centrifugal end, pour out throw out, repeatedly alcohol wash, centrifugal 3 times.Add the distilled water of 3 times of volumes in throw out after centrifugal to alcohol wash again, the centrifugal 10min of the rotating speed through 6000rpm, pours out throw out after centrifugal end, repeatedly washes, after centrifugal 3 times, is separated the jelly precipitation obtained and is nano-cellulose (see Fig. 2).Obtain nano-cellulose through phospho-wolframic acid hydrolysis wood pulps as seen from Figure 2, its particle diameter is the rhabdolith of 15-40nm nano-scale.
Embodiment 2
Take 0.5g Microcrystalline Cellulose and be placed in round-bottomed flask, add 20ml70% (w/w) phosphotungstic acid aqueous solution, at 90 DEG C, 18h is stirred with the speed mechanical of 4500rpm, after having reacted, rapid ice bath to room temperature, with reaction solution: ether is that the volume ratio of 1:4 adds ether, extracting twice, lower floor's phospho-wolframic acid ether extraction liquid reclaims, and through 35 DEG C, vacuum tightness isolates phospho-wolframic acid solid for-0.5MPa rotary evaporation, ether reclaims through condensing works, phospho-wolframic acid and the equal reusable edible of ether; The ethanol of 2 times of volumes is added in the nanofiber cellulose solution of upper strata, be stirred to glass stick and mix, with the centrifugal 10min of the rotating speed of 6000rpm, throw out is poured out after centrifugal end, the ethanol adding 2 times of volumes in throw out mixes, with the centrifugal 10min of the rotating speed of 6000rpm, after centrifugal end, pour out throw out, repeatedly alcohol wash, centrifugal 3 times.Add the distilled water of 2 times of volumes in throw out after centrifugal to alcohol wash again, the centrifugal 10min of the rotating speed through 6000rpm, pours out throw out after centrifugal end, repeatedly washes, after centrifugal 3 times, is separated the jelly precipitation obtained and is nano-cellulose (see Fig. 4).Phospho-wolframic acid hydrolyzing microcrystalline cellulose as seen from Figure 4, its particle diameter is the rhabdolith of 15-40nm nano-scale.
Embodiment 3
By in embodiment 1 through rotary evaporation Separation and Recovery phospho-wolframic acid solid, in the baking oven of 40 DEG C, dry 24h, stand-by.Take 0.5g wood pulps and be placed in round-bottomed flask, by water-soluble for the phospho-wolframic acid of the recovery phosphotungstic acid aqueous solution being made into 75% (w/w), get 20ml to add in round-bottomed flask and mix with wood pulps, at 90 DEG C, mechanical stirring 30h, after having reacted, rapid ice bath is to room temperature, with reaction solution: ether is that the volume ratio of 1:3 adds ether, extracting twice, lower floor's phospho-wolframic acid ether extraction liquid reclaims, through 35 DEG C, vacuum tightness isolates phospho-wolframic acid solid for-0.5MPa rotary evaporation, and ether is through condensing works recycle and reuse; The ethanol of 3 times of volumes is added in the nanofiber cellulose solution of upper strata, be stirred to glass stick and mix, with the centrifugal 10min of the rotating speed of 6000rpm, throw out is poured out after centrifugal end, the ethanol adding 3 times of volumes in throw out mixes, with the centrifugal 10min of the rotating speed of 6000rpm, after centrifugal end, pour out throw out, repeatedly alcohol wash, centrifugal 3 times.Add the distilled water of 3 times of volumes in throw out after centrifugal to alcohol wash again, the centrifugal 10min of the rotating speed through 6000rpm, pours out throw out after centrifugal end, repeatedly washes, after centrifugal 3 times, is separated the jelly precipitation obtained and is nano-cellulose (see Fig. 5).The rhabdolith of the nano-cellulose of phospho-wolframic acid hydrolysis obtained by wood pulps of recycling use to be its particle diameter be 15-40nm nano-scale as seen from Figure 5.
Claims (7)
1. prepare a method for nano-cellulose, it is characterized in that:
1) phospho-wolframic acid hydrolysis fiber cellulose fiber: be added to the water by cellulose fiber peacekeeping phospho-wolframic acid powder, heated and stirred obtains hydrolysis fiber cellulose fiber;
2) be separated, purifying and recycle: in above-mentioned hydrocellulose fiber, add extraction agent, extraction collects the upper and lower liquid respectively, and upper liquid obtains nano cellulose crystal through alcohol wash, washing, centrifugal and freezing dry process; Subnatant underpressure distillation is reclaimed and is collected extraction agent and Powdered phospho-wolframic acid and then cycling and reutilization respectively.
2. by the method preparing nano-cellulose according to claim 1, it is characterized in that: solid-liquid ratio is that the cellulosic fibre of 1:40-80 and phosphotungstic acid aqueous solution are added to the water by described step 1), at 50 DEG C-90 DEG C, stir 15h-50h with the speed of 4000rpm-5000rpm; Wherein the mass concentration of phospho-wolframic acid in water is 50%-80%.
3. by the method preparing nano-cellulose described in claim 1 or 2, it is characterized in that: described cellulosic fibre is one or both of wood pulps, Cotton Pulp, straw pulp or Microcrystalline Cellulose.
4. by the method preparing nano-cellulose according to claim 1, it is characterized in that: described step 2) said hydrolyzed cellulosic fibre is mixed with the volume ratio of extraction agent according to 1:3-1:5, repeatedly extract 2-5 time, merge upper liquid and the subnatant of each time, upper liquid amasss 1-3 water washing doubly 3-5 time, then with the speed of 2000rpm-12000rpm with supernatant liquid again after upper liquid volume 1-3 alcohol alcohol wash 3-5 time doubly, alcohol wash; Centrifugal 3-5 time, each 10min-20min, obtains nano cellulose crystal finally by lyophilize; Subnatant 35 DEG C-45 DEG C, vacuum tightness be-0.5MPa ~ 0.1MPa under underpressure distillation reclaim and collect extraction agent and Powdered phospho-wolframic acid and then cycling and reutilization respectively.
5. by the method preparing nano-cellulose described in claim 1 or 4, it is characterized in that: described catalyzer is ether.
6. by the method preparing nano-cellulose described in claim 1 or 4, it is characterized in that: the Powdered phospho-wolframic acid drying that described underpressure distillation is reclaimed is reusable edible afterwards.
7. by the method preparing nano-cellulose described in claim 1 or 4, it is characterized in that: described alcohol can be one or more mixing in ethanol, methyl alcohol or butanols.
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Cited By (10)
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| CN105153316A (en) * | 2015-10-19 | 2015-12-16 | 中国科学院青岛生物能源与过程研究所 | Method for preparing nano cellulose by formic acid hydrolysis by using metal salt catalyst |
| CN105419787A (en) * | 2015-12-22 | 2016-03-23 | 华南理工大学 | Purification method in post treatment of cellulose-based rare earth luminescent material preparation |
| CN105713099A (en) * | 2016-01-21 | 2016-06-29 | 中国科学院青岛生物能源与过程研究所 | Method combining formic acid preprocessing and high-pressure homogenization to prepare nano-crystalline cellulose fibrils |
| CN108219007A (en) * | 2018-01-17 | 2018-06-29 | 天津科技大学 | A kind of preparation method of the Cellulose nanocrystal of solid fossil matter acid-catalyzed hydrolysis |
| WO2018157453A1 (en) * | 2017-03-03 | 2018-09-07 | 曾济天 | Nanocellulose, preparation method therefor, and application thereof |
| CN109594384A (en) * | 2018-12-21 | 2019-04-09 | 太原理工大学 | A method of microcrystalline cellulose is prepared using waste cotton fabric |
| TWI684693B (en) * | 2018-06-08 | 2020-02-11 | 行政院原子能委員會核能研究所 | Method of Fabricating Nanoscaled Cellulose with Ionic Liquid Heteropolyacid Catalyst |
| CN112618455A (en) * | 2020-12-31 | 2021-04-09 | 重庆知翔科技有限公司 | Moisture mask and preparation method thereof |
| CN112641704A (en) * | 2020-12-31 | 2021-04-13 | 重庆知翔科技有限公司 | Moisturizing composition and preparation method thereof |
| CN113087924A (en) * | 2021-04-13 | 2021-07-09 | 华纺股份有限公司 | Method for preparing nano cellulose suspension by low-temperature hydrothermal method |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105153316A (en) * | 2015-10-19 | 2015-12-16 | 中国科学院青岛生物能源与过程研究所 | Method for preparing nano cellulose by formic acid hydrolysis by using metal salt catalyst |
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| CN105419787A (en) * | 2015-12-22 | 2016-03-23 | 华南理工大学 | Purification method in post treatment of cellulose-based rare earth luminescent material preparation |
| CN105419787B (en) * | 2015-12-22 | 2018-06-12 | 华南理工大学 | A kind of cellulose base rare earth luminescent material prepares the method for purification in post processing |
| CN105713099A (en) * | 2016-01-21 | 2016-06-29 | 中国科学院青岛生物能源与过程研究所 | Method combining formic acid preprocessing and high-pressure homogenization to prepare nano-crystalline cellulose fibrils |
| WO2018157453A1 (en) * | 2017-03-03 | 2018-09-07 | 曾济天 | Nanocellulose, preparation method therefor, and application thereof |
| CN108219007A (en) * | 2018-01-17 | 2018-06-29 | 天津科技大学 | A kind of preparation method of the Cellulose nanocrystal of solid fossil matter acid-catalyzed hydrolysis |
| TWI684693B (en) * | 2018-06-08 | 2020-02-11 | 行政院原子能委員會核能研究所 | Method of Fabricating Nanoscaled Cellulose with Ionic Liquid Heteropolyacid Catalyst |
| CN109594384A (en) * | 2018-12-21 | 2019-04-09 | 太原理工大学 | A method of microcrystalline cellulose is prepared using waste cotton fabric |
| CN109594384B (en) * | 2018-12-21 | 2021-05-28 | 太原理工大学 | Method for preparing microcrystalline cellulose by using waste cotton fabric |
| CN112618455A (en) * | 2020-12-31 | 2021-04-09 | 重庆知翔科技有限公司 | Moisture mask and preparation method thereof |
| CN112641704A (en) * | 2020-12-31 | 2021-04-13 | 重庆知翔科技有限公司 | Moisturizing composition and preparation method thereof |
| CN113087924A (en) * | 2021-04-13 | 2021-07-09 | 华纺股份有限公司 | Method for preparing nano cellulose suspension by low-temperature hydrothermal method |
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