CN103643577A - Method for preparation of nano-cellulose whiskers from garlic skins - Google Patents
Method for preparation of nano-cellulose whiskers from garlic skins Download PDFInfo
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- CN103643577A CN103643577A CN201310610082.7A CN201310610082A CN103643577A CN 103643577 A CN103643577 A CN 103643577A CN 201310610082 A CN201310610082 A CN 201310610082A CN 103643577 A CN103643577 A CN 103643577A
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- 229920002678 cellulose Polymers 0.000 title claims abstract description 45
- 239000001913 cellulose Substances 0.000 title claims abstract description 45
- 235000004611 garlic Nutrition 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 244000245420 ail Species 0.000 title 1
- 240000002234 Allium sativum Species 0.000 claims abstract description 31
- 238000005406 washing Methods 0.000 claims abstract description 21
- 238000004061 bleaching Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 150000004676 glycans Chemical class 0.000 claims abstract description 10
- 229920001282 polysaccharide Polymers 0.000 claims abstract description 10
- 239000005017 polysaccharide Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000502 dialysis Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000004108 freeze drying Methods 0.000 claims abstract description 6
- 230000008961 swelling Effects 0.000 claims abstract description 6
- 239000006185 dispersion Substances 0.000 claims abstract description 5
- 230000020477 pH reduction Effects 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 239000004576 sand Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000000284 extract Substances 0.000 claims description 8
- 238000002386 leaching Methods 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 6
- 238000003801 milling Methods 0.000 claims description 6
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical group [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 230000002776 aggregation Effects 0.000 claims description 4
- 238000004220 aggregation Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000000413 hydrolysate Substances 0.000 claims description 4
- 238000011034 membrane dialysis Methods 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 3
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims description 2
- 239000005416 organic matter Substances 0.000 claims description 2
- 150000008442 polyphenolic compounds Chemical class 0.000 claims description 2
- 235000013824 polyphenols Nutrition 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 239000003643 water by type Substances 0.000 claims description 2
- 238000001238 wet grinding Methods 0.000 claims description 2
- 239000007844 bleaching agent Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000005291 magnetic effect Effects 0.000 abstract description 3
- 230000007062 hydrolysis Effects 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- 239000001814 pectin Substances 0.000 abstract description 2
- 229920001277 pectin Polymers 0.000 abstract description 2
- 235000010987 pectin Nutrition 0.000 abstract description 2
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract 2
- 239000003513 alkali Substances 0.000 abstract 1
- 238000013329 compounding Methods 0.000 abstract 1
- 238000010411 cooking Methods 0.000 abstract 1
- 238000007598 dipping method Methods 0.000 abstract 1
- 238000000605 extraction Methods 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract 1
- 239000000047 product Substances 0.000 description 13
- 238000000967 suction filtration Methods 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 239000000835 fiber Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 241000589220 Acetobacter Species 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 229920002522 Wood fibre Polymers 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- -1 stalk Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to a method for preparation of nano-cellulose whiskers from garlic skins. Taking garlic skins as raw materials, the method includes the steps of: 1) conducting dipping swelling in a sodium carbonate solution; 2) performing cooking degumming by an alkali solution; 3) carrying out polysaccharide extraction; 4) implementing bleaching treatment; 5) conducting sanding treatment; 6) performing acidification hydrolysis; and 7) carrying out washing dialysis and freeze drying, etc. The garlic skin raw materials undergo component separation and conversion to be made into a nano-cellulose dispersion liquid with certain concentration, and the dispersion liquid is subjected to freeze drying to remove water, thus obtaining the nano-cellulose whiskers. The nano-cellulose whiskers prepared by the method provided by the invention is needle-shaped, presents good dispersion, and has a high length-diameter ratio, a diameter of 20nm-30nm, and a length of 300nm-2micrometers. The method provided by the invention adopts garlic skins as the raw materials to remove pectin and other impurities. After functional compounding, the prepared nano-cellulose whiskers have wide application value in the fields of optics, electrics, magnetics, biology and semiconductors, etc.
Description
Technical field
The present invention relates to a kind of preparation method of nano-cellulose, particularly a kind of method of utilizing garlic skin to prepare nano-cellulose whisker.
Background technology
In recent years, the non-renewable energy resources such as natural gas, coal, oil all face in short supply.Be accompanied by economic fast development, the great demand of the energy is produced to tremendous influence to World Economics.In export growth, the development model of highly energy-consuming high pollution also becomes the theme of people's worry day by day.In order to address this problem, must strengthen exploitation and the use dynamics of new forms of energy, could, meeting under the development prerequisite of recycling economy, better carry out environmental protection like this.
Cellulose is one of the abundantest natural polymers of occurring in nature, it is the main chemical composition of plant fiber material, also be for paper pulp and main, the most basic component of papermaking, renewable resource as nature biotechnology reserves are maximum, biocompatibility is remarkable, prospect is fabulous, has very large application potential.Nano-cellulose is the ultra tiny fiber that diameter is less than 100 nm, also be cellulosic minimal physical construction unit, nano-cellulose has many good characteristics, as high-crystallinity, high-purity, high Young's modulus, high strength, high-hydrophilic, hyperfine structure and high transparent etc., can obviously change the optics of material, electricity, magnetics, rheological property, insulating properties and superconductivity, and there is native cellulose lightweight, degradable, bio-compatible and the characteristic such as renewable, it is in papermaking, building, automobile, food, cosmetics, electronic product, there is huge potential application foreground in the fields such as medical science.
The Garlic yield of China is very high, and long-term cultivated area is 20.0 ~ 26.7 ten thousand hectares, and output is 4,000,000 tons, occupies first place in the world, and accounts for 1/4 of Gross World Product.In daily life, garlic skin, generally with house refuse or the formal layout that burns, cannot be accomplished the recycling of resource, has also aggravated to a certain extent the impact of greenhouse effects simultaneously.The main component of garlic skin is pectin and cellulose.With from the material such as wood fibre, stalk, extract cellulose Comparatively speaking, utilize garlic skin to extract the process that cellulose has been avoided delignification, this has not only saved reaction raw materials, has also also reduced to a certain extent and has polluted the ambient influnence bringing.
Prepare at present and in the method for nano-cellulose, also do not utilize directly preparation of garlic skin, and there is in the separation for the many strings of this gum level a difficult problem that is difficult to capture in prior art, and the nano-cellulose that preparation draw ratio is high is many to be made by the acetobacter fiber of manually cultivating, technique is loaded down with trivial details, take time and effort, limited Application of composite and the development of high length-diameter ratio nano-cellulose whisker.
Summary of the invention
The object of the invention is to overcome problems of the prior art, a kind of method of utilizing garlic skin to prepare nano-cellulose is provided.
For achieving the above object, the present invention adopts following technical scheme:
Utilize garlic skin to prepare a method for nano-cellulose, it is characterized in that the concrete steps of the method are:
A. high pressure swelling: 1 ~ 5 g garlic skin is inserted in autoclave, and adding 50 ~ 300 g mass percent concentrations is the Na of 2 ~ 4 wt%
2cO
3the aqueous solution, it is baking oven 120 min of 100 ~ 120 ℃ that autoclave is placed in to temperature, crosses leaching residue washing and drains to neutrality;
B. boiling is come unstuck: by step a gained filter residue add 50 ~ 150 g mass percent concentrations be the NaOH aqueous solution of 2 ~ 5 wt% except glue, in temperature, be boiling 2 ~ 4 h in the oil bath of 110 ~ 125 ℃, cross leaching residue washing and drain to neutrality;
C. polysaccharide extracts: it is 2wt% H that step b gained filter residue is adopted to 300 ~ 500 mL mass percent concentrations
2sO
4solution stirs 2 ~ 3h and removes solubility in acid polysaccharide and Polyphenols organic matter at 90 ℃, crosses leaching residue washing and drains to neutrality;
D. bleaching: step c gained filter residue is carried out to bleaching, through H
2o
2and NaClO
2solution is bleached after a period of time successively, crosses leaching residue washing and drains to neutrality;
E. sanded treatment: steps d gained filter residue is added in sand milling tank to ultrasonic dispersion 1 ~ 2 h again after wet-milling under high rotating speed, the vacuumize in vacuum drying oven of gained dispersion liquid;
F. acidification hydrolization: it is 45 ~ 50 wt% sulfuric acid that step e gained sample is added to mass percent concentration, the mass ratio of acid and sample is 9 ~ 10, in temperature, is at 45 ~ 55 ℃, to be hydrolyzed 2 ~ 8 h, then adds a large amount of deionized waters to dilute with cessation reaction;
G. wash dialysis/freeze drying: by step f gained hydrolysate deionized water centrifuge washing, adopt dialysis membrane dialysis to neutral, ultrasonic 30min in suspension water-bath, filters and remove aggregation; Nano-cellulose whisker colloidal solution liquid nitrogen frozen by obtaining dewaters and can make nano-cellulose whisker in freeze drier.
Above-mentioned bleaching process: it is 5wt% H that the product that extracts polysaccharide is added to 400 mL mass percents
2o
2in solution, with NaOH adjust pH to 11.5,45 ℃ of stirring reaction 5 ~ 8 h of oil bath, are then cooled to room temperature, then to adopt 300 mL mass percents be 1.4wt% acidifying NaClO
2solution continues bleaching, uses CH
3cOOH adjusts pH to 3.0 – 4.0, under 70 ~ 90 ℃ of conditions of temperature, bleaches 2 ~ 4 h.
Above-mentioned sanded treatment condition: in sand mill, add sample 5 g that process through steps d, water 200 mL, diameter is zirconium pearl quality 600 ~ 800g of 3 μ m, sand milling 1 ~ 2 h under the rotating speed of 2000 ~ 3500r/min.
The preparation method of garlic skin nano-cellulose of the present invention has following advantage:
(1) utilize the inventive method rationally efficiently to utilize house refuse garlic skin, when avoiding the impact of ecological environment and harm, produce economic benefit;
(2) utilize the nano-cellulose whisker that the inventive method makes to become needle-like, diameter 20nm ~ 30nm, length 300nm ~ 2 μ m, draw ratio is high, and specific area is large, has advantages of that mechanical performance is high, good biocompatibility, composite reactive be high;
(3) having solved prior art is difficult to utilize plant to prepare the problem of high length-diameter ratio, high mechanical properties nano-cellulose whisker;
(4) technique is simple, easy to implement, and consuming little energy, production cost are low, in preparation process, do not produce environment harmful side product, and productive rate is higher;
(5) gained nano-cellulose whisker can be dispersed in the multi-solvents such as water, ethanol, and the fields such as optics, electricity, magnetics, biology and semiconductor that are compounded in through functionalization are with a wide range of applications.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of the garlic skin nano-cellulose of specific embodiment one preparation;
Fig. 2 is the transmission electron microscope photo of the garlic skin nano-cellulose of specific embodiment two preparations;
Fig. 3 is the transmission electron microscope photo of the garlic skin nano-cellulose of specific embodiment three preparations.
The specific embodiment
Below in conjunction with embodiment, the present invention is described in detail:
embodiment mono-:concrete steps are as follows:
(1) high pressure swelling: 2g garlic skin is inserted in autoclave, and adding 100g mass percent concentration is the Na of 2wt%
2cO
3the aqueous solution, it is baking oven 120 min of 120 ℃ that autoclave is placed in to temperature, by mixture suction filtration/washing; (2) boiling is come unstuck: will insert in reaction vessel through the product of swelling suction filtration, adding 100g mass percent concentration is the NaOH aqueous solution of 4 wt%, is to react 4 h in 120 ℃ of oil baths, by mixture suction filtration/washing in temperature; (3) polysaccharide extracts: the product fiber coming unstuck is inserted to the H that 400 mL mass fractions are 2%
2sO
4in the aqueous solution, in temperature, be stirring reaction 2 h in 90 ℃ of oil baths, suction filtration/washing again; (4) bleaching: the product that extracts polysaccharide is added to 400 mL 5wt% H
2o
2in solution, with NaOH adjust pH to 11.5,45 ℃ of stirring reaction 6 h of oil bath, are then cooled to room temperature, adopt 300 mL 1.4wt% acidifying NaClO
2solution continues bleaching, uses CH
3cOOH adjusts pH to 3.0 ~ 4.0,80 ℃ of stirring bleaching 2 h of oil bath; (5) sanded treatment: the product after bleaching is placed in to sand mill, adds water 200 mL, diameter is zirconium pearl quality 600 ~ 800g of 3 μ m, sand milling 1 h under the rotating speed of 2500 r/min, products therefrom is placed in vacuum drying oven vacuumize; (6) acidification hydrolization: it is 50 wt% sulfuric acid that the sample that vacuumize is obtained adds mass percent concentration, the mass ratio of acid and sample is 10, the oil bath that is 50 ℃ in temperature is hydrolyzed 5 h; (7) washing dialysis/freeze drying: by gained hydrolysate deionized water centrifuge washing, adopt dialysis membrane dialysis to neutral, ultrasonic 30min in suspension water-bath, filters and remove aggregation.Nano-cellulose colloidal solution liquid nitrogen frozen by obtaining dewaters and can make nano-cellulose in freeze drier.
As shown in Figure 1, as can be seen from Fig., garlic skin nano-cellulose whisker is needle-like to the transmission electron microscope photo of garlic skin nano-cellulose whisker prepared by present embodiment, and diameter is 20 nm ~ 30 nm, and length is 300 nm ~ 2 μ m.
embodiment bis-:concrete steps are as follows:
(1) digesting and screening: 4 g garlic skins are inserted in autoclave, add the Na that 200 g mass percent concentrations are 2wt%
2cO
3the aqueous solution, it is baking oven 120 min of 120 ℃ that autoclave is placed in to temperature, by mixture suction filtration/washing; (2) boiling is come unstuck: will insert in reaction vessel through the product of swelling suction filtration, adding 200g mass percent concentration is the NaOH aqueous solution of 5 wt%, is to react 4 h in 120 ℃ of oil baths, by mixture suction filtration/washing in temperature; (3) polysaccharide extracts: the product fiber coming unstuck is inserted to the H that 600 mL mass fractions are 2%
2sO
4in the aqueous solution, in temperature, be stirring reaction 2 h in 90 ℃ of oil baths, suction filtration/washing again; (4) bleaching: the product that extracts polysaccharide is added to 400 mL 5wt% H
2o
2in solution, with NaOH adjust pH to 11.5,45 ℃ of stirring reaction 6 h of oil bath, are then cooled to room temperature, adopt 300 mL 1.4wt% acidifying NaClO
2liquid continues bleaching, uses CH
3cOOH adjusts pH to 3.0 ~ 4.0, under 80 ℃ of conditions of oil bath, bleaches 2 h; (5) sanded treatment: the product after bleaching is placed in to sand mill, adds water 200 mL, diameter is zirconium pearl quality 600 ~ 800g of 3 μ m, sand milling 1 h under the rotating speed of 2500 r/min, products therefrom is placed in vacuum drier vacuumize; (6) acidification hydrolization: it is 50 wt% sulfuric acid that the sample that vacuumize is obtained adds mass percent concentration, the mass ratio of acid and sample is 10, the oil bath that is 50 ℃ in temperature is hydrolyzed 5 h; (7) washing dialysis/freeze drying: by gained hydrolysate deionized water centrifuge washing, adopt dialysis membrane dialysis to neutral, ultrasonic 30min in suspension water-bath, filters and remove large stretch of aggregation.Nano-cellulose colloidal solution liquid nitrogen frozen by obtaining dewaters and can make nano-cellulose in freeze drier.
As shown in Figure 2, as can be seen from the figure, garlic skin nano-cellulose whisker is needle-like to the transmission electron microscope photo of garlic skin nano-cellulose whisker prepared by present embodiment, and diameter is 20nm ~ 30nm, and length is 300nm ~ 2 μ m.
embodiment tri-:concrete steps are as follows: the present embodiment and embodiment bis-are basic identical, and difference is: in sulfuric acid solution, stir hydrolysis 8 h.
As shown in Figure 3, as seen from the figure, garlic skin nano-cellulose whisker is needle-like to the transmission electron microscope photo of garlic skin nano-cellulose prepared by present embodiment, and diameter is 20nm ~ 30nm, and length is 300nm ~ 2 μ m.
Those of ordinary skill in the art can be easy to these embodiments to make various modifications, and general application of principle described herein in other application example and needn't pass through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and the improvement that the present invention is made and modification all should be within protection scope of the present invention.
Claims (3)
1. utilize garlic skin to prepare a method for nano-cellulose whisker, it is characterized in that the concrete steps of the method are:
A. high pressure swelling: 1 ~ 5 g garlic skin is inserted in autoclave, and adding 50 ~ 300 g mass percent concentrations is the Na of 2 ~ 4 wt%
2cO
3the aqueous solution, it is baking oven 120 min of 100 ~ 120 ℃ that autoclave is placed in to temperature, crosses leaching residue washing and drains to neutrality;
B. boiling is come unstuck: by step a gained filter residue add 50 ~ 150 g mass percent concentrations be the NaOH aqueous solution of 2 ~ 5 wt% except glue, in temperature, be boiling 2 ~ 4 h in the oil bath of 110 ~ 125 ℃, cross leaching residue washing and drain to neutrality;
C. polysaccharide extracts: it is 2wt% H that step b gained filter residue is adopted to 300 ~ 500 mL mass percent concentrations
2sO
4solution stirs 2 ~ 3h and removes solubility in acid polysaccharide and Polyphenols organic matter at 90 ℃, crosses leaching residue washing and drains to neutrality;
D. bleaching: step c gained filter residue is carried out to bleaching, through H
2o
2and NaClO
2solution is bleached after a period of time successively, crosses leaching residue washing and drains to neutrality;
E. sanded treatment: steps d gained filter residue is added in sand milling tank to ultrasonic dispersion 1 ~ 2 h again after wet-milling under high rotating speed, the vacuumize in vacuum drying oven of gained dispersion liquid;
F. acidification hydrolization: it is 45 ~ 50 wt% sulfuric acid that step e gained sample is added to mass percent concentration, the mass ratio of acid and sample is 9 ~ 10, in temperature, is at 45 ~ 55 ℃, to be hydrolyzed 2 ~ 8 h, then adds a large amount of deionized waters to dilute with cessation reaction;
G. wash dialysis/freeze drying: by step f gained hydrolysate deionized water centrifuge washing, adopt dialysis membrane dialysis to neutral, ultrasonic 30min in suspension water-bath, filters and remove aggregation; Nano-cellulose whisker colloidal solution liquid nitrogen frozen by obtaining dewaters and can make nano-cellulose whisker in freeze drier.
2. the method for utilizing garlic skin to prepare nano-cellulose whisker according to claim 1, is characterized in that described bleaching process: the H that 400 mL mass percent concentrations are 5wt%
2o
2with NaOH adjust pH to 11.5,45 ℃ are stirred 5 ~ 8 h, are then cooled to room temperature, and adopting 300 mL mass percent concentrations is 1.4wt% acidifying NaClO
2solution continues bleaching, uses CH
3cOOH adjusts pH to 3.0 – 4.0, in temperature, is to bleach 2 ~ 4 h under 70 ~ 90 ℃ of conditions.
3. garlic skin according to claim 1 is prepared the method for nano-cellulose whisker, it is characterized in that sanded treatment condition: in sand mill, add sample 5 g that process through steps d, water 200 mL, diameter is zirconium pearl 600 ~ 800g of 2 ~ 3 μ m, sand milling 1 ~ 2 h under the rotating speed of 2000 ~ 3500r/min.
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| CN103952941A (en) * | 2014-05-08 | 2014-07-30 | 临沂市清宇环境资源综合利用研究院 | Method for manufacturing pulp by using garlic slices |
| 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 |
| CN104762845A (en) * | 2015-04-13 | 2015-07-08 | 东华大学 | Method for extracting cellulose nanowhiskers from corn husks |
| CN104762846A (en) * | 2015-04-13 | 2015-07-08 | 东华大学 | Preparation method of cotton-straw peel cellulose nanowhiskers |
| CN104805723A (en) * | 2015-04-13 | 2015-07-29 | 东华大学 | Etherification and oxidization method for preparing cellulose nano crystal whiskers |
| CN104805722A (en) * | 2015-04-13 | 2015-07-29 | 东华大学 | Method for preparing straw cellulose nano crystal whisker |
| CN105601754A (en) * | 2016-01-06 | 2016-05-25 | 扬州大学 | Preparing method for acylated fiber nanocrystal |
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| CN106480765A (en) * | 2016-10-19 | 2017-03-08 | 天津中智科技发展有限公司 | A kind of preparation method of Lignum seu Ramulus Cunninghamiae Lanceolatae nanofiber |
| CN109881521A (en) * | 2017-12-06 | 2019-06-14 | 山东省圣泉生物质石墨烯研究院 | A kind of nano-cellulose, Preparation method and use |
| CN115926012A (en) * | 2022-11-21 | 2023-04-07 | 重庆市天友乳业股份有限公司 | Garlic skin modified polysaccharide and preparation method and application thereof |
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