CN117362457A - Green efficient preparation method of nanocellulose - Google Patents
Green efficient preparation method of nanocellulose Download PDFInfo
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- CN117362457A CN117362457A CN202311343654.XA CN202311343654A CN117362457A CN 117362457 A CN117362457 A CN 117362457A CN 202311343654 A CN202311343654 A CN 202311343654A CN 117362457 A CN117362457 A CN 117362457A
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- 229920001046 Nanocellulose Polymers 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 55
- 229920002678 cellulose Polymers 0.000 claims abstract description 82
- 239000001913 cellulose Substances 0.000 claims abstract description 82
- 238000000227 grinding Methods 0.000 claims abstract description 46
- 239000007788 liquid Substances 0.000 claims abstract description 40
- 239000006185 dispersion Substances 0.000 claims abstract description 36
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 235000010980 cellulose Nutrition 0.000 claims description 79
- 238000000034 method Methods 0.000 claims description 23
- 238000009210 therapy by ultrasound Methods 0.000 claims description 18
- 239000002270 dispersing agent Substances 0.000 claims description 15
- 239000002159 nanocrystal Substances 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- 239000006228 supernatant Substances 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 7
- 238000003828 vacuum filtration Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 4
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 4
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 4
- 239000011425 bamboo Substances 0.000 claims description 4
- 235000004431 Linum usitatissimum Nutrition 0.000 claims description 3
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 3
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 3
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 3
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 3
- 241001474374 Blennius Species 0.000 claims 1
- 240000006240 Linum usitatissimum Species 0.000 claims 1
- 244000082204 Phyllostachys viridis Species 0.000 claims 1
- 239000002894 chemical waste Substances 0.000 abstract description 6
- 238000007781 pre-processing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 241001330002 Bambuseae Species 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 3
- 108010059892 Cellulase Proteins 0.000 description 3
- 229940106157 cellulase Drugs 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- GDOPTJXRTPNYNR-UHFFFAOYSA-N methyl-cyclopentane Natural products CC1CCCC1 GDOPTJXRTPNYNR-UHFFFAOYSA-N 0.000 description 3
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 241000208202 Linaceae Species 0.000 description 2
- 108010059820 Polygalacturonase Proteins 0.000 description 2
- 239000005708 Sodium hypochlorite Substances 0.000 description 2
- 229940072056 alginate Drugs 0.000 description 2
- 229920000615 alginic acid Polymers 0.000 description 2
- 235000010443 alginic acid Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010170 biological method Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229940088598 enzyme Drugs 0.000 description 2
- 108010093305 exopolygalacturonase Proteins 0.000 description 2
- 238000010297 mechanical methods and process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 2
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000007073 chemical hydrolysis Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/08—Fractionation of cellulose, e.g. separation of cellulose crystallites
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention provides a green efficient preparation method of nanocellulose, which relates to the technical field of nanocellulose and comprises the following steps: s1, preprocessing a cellulose raw material; s2, preparing cellulose dispersion liquid; s3, mechanically grinding; and S4, centrifugal separation. The green efficient preparation method of the nanocellulose can safely, quickly, green and efficiently prepare the nanocellulose, has high preparation efficiency and yield, low preparation cost and no chemical waste liquid, and can realize large-scale mass production.
Description
Technical Field
The invention relates to the technical field of nanocellulose, in particular to a green efficient preparation method of nanocellulose.
Background
Nanocellulose is a nanoscale product obtained by processing cellulose fibers. Compared with the traditional cellulose material, the nano cellulose has the characteristics of large specific surface area, large crystallinity, large tensile strength, high modulus, biodegradability, light weight and the like, is considered to be the most promising composite material reinforcement, and has wide market space in various fields of environmental protection, papermaking, packaging, food, energy, composite material, medicine and the like. With the further widening of the application range, the demand for nanocellulose is increasing, and the performance requirement is also increasing.
At present, the preparation of the nanocellulose mainly adopts an acid method, a mechanical method, a TEMPO oxidation method, a sodium hypochlorite method or a biological method. The acid solution of the nano cellulose prepared by the acid method is easy to cause environmental pollution when discharged after reaction; the nanocellulose prepared by a mechanical method has low yield, and all used equipment has high energy consumption; the TEMPO oxidation or sodium hypochlorite method for preparing nano cellulose is the same as the acid method, is easy to cause environmental pollution and has high TEMPO price. The biological method for preparing the nanocellulose has low production efficiency.
In order to solve the problems, the Chinese patent application No. 202110764892.2 discloses a preparation method of green efficient nanocellulose, which comprises the following steps: mixing biomass cellulose, a cellulose aqueous solution and a pectinase aqueous solution for enzymolysis treatment; the mass ratio of the total mass of the aqueous cellulase solution and the aqueous pectase solution to the biomass cellulose is (15-30): 1, the enzyme activity of the cellulase in the aqueous cellulase solution is 30-150U/mL, the enzyme activity of the pectase in the aqueous pectase solution is 300-1500U/mL, and the enzymolysis treatment time is 15-60 min. According to the preparation method of the nanocellulose, the biomass cellulose is treated by adopting the cellulose aqueous solution and the pectinase aqueous solution together, so that the production efficiency and the yield of the nanocellulose are remarkably improved, and the nanocellulose is environment-friendly. However, the preparation method still has the technical defects of higher price, chemical waste liquid generation and the like.
Therefore, the development of the green efficient preparation method of the nanocellulose, which can safely, quickly, green and efficiently prepare nanocellulose, has the advantages of high preparation efficiency and yield, low preparation cost and no chemical waste liquid, can realize large-scale mass production, meets the market demand, has wide market value and application prospect, and has very important significance in promoting the further development of the nanocellulose field.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the green and efficient preparation method of the nanocellulose, which can safely, quickly, green and efficiently prepare the nanocellulose, has high preparation efficiency and yield, low preparation cost and no chemical waste liquid, and can realize large-scale mass production.
The invention can be realized by the following technical scheme:
the invention relates to a green efficient preparation method of nanocellulose, which comprises the following steps:
step S1, pretreatment of cellulose raw materials: cutting cellulose raw material into powder by a dry method at high frequency;
step S2, preparation of cellulose dispersion liquid: adding the cellulose powder prepared in the step S1 into a dispersing agent, and uniformly dispersing to prepare cellulose dispersion liquid;
step S3, mechanical grinding: grinding the cellulose dispersion liquid prepared in the step S2 in a P7 miniature planetary high-energy ball mill for 1-2h;
step S4, centrifugal separation: and (3) separating the dispersion liquid obtained through the treatment in the step (S3) by adopting a centrifugal machine to obtain supernatant containing cellulose nanocrystals, and then carrying out vacuum filtration and defoaming on the supernatant to prepare the cellulose nanocrystals.
Preferably, the powder in step S1 has a width in the range of 8 to 20 μm and a length in the range of 20 to 50. Mu.m.
Preferably, the cellulose raw material in the step S1 is any one of bamboo cellulose, flax cellulose, alginate cellulose and microcrystalline cellulose which is artificially treated.
Preferably, the dispersant in step S2 is at least one of water and ethanol.
Preferably, the mass percentage concentration of the cellulose dispersion in step S2 is 0.5wt% to 5.5wt%.
Preferably, the grinding in step S3 is batch grinding, and each grinding time is 15min and 10min.
Preferably, the mechanical grinding in step S3 is preceded by ultrasonic treatment, microwave treatment and magnetic field treatment.
Preferably, the ultrasonic treatment frequency is 50-80kHz, the power range is 400-800W, and the treatment time is 15-35min.
Preferably, the microwave treatment frequency is 2.2-2.5GHz, the power range is 600-1300W, and the treatment time is 5-20min.
Preferably, the magnetic field strength of the magnetic field treatment is 7500-16500Gs, and the treatment time is 10-25min.
Preferably, the centrifuge in step S4 is controlled to have a rotational speed of 3500 to 7500rpm during centrifugation.
The invention further aims at providing the nanocellulose prepared by the nanocellulose green efficient preparation method.
Compared with the prior art, the invention has the beneficial effects that:
(1) The green efficient preparation method of the nanocellulose disclosed by the invention can safely, quickly, green and efficiently prepare the nanocellulose, has high preparation efficiency and yield, low preparation cost and no chemical waste liquid, can realize large-scale mass production, and has higher popularization and application values.
(2) The green efficient preparation method of the nanocellulose disclosed by the invention adopts a solid-phase mechanochemical grinding preparation technology, and is different from the traditional chemical hydrolysis method, wherein the technology adopts a pure physical grinding method, so that no chemical waste liquid is generated, the production efficiency is high, the cost is low, and the large-scale mass production can be realized.
(3) According to the green efficient preparation method of the nanocellulose, disclosed by the invention, before mechanical grinding, ultrasonic treatment, microwave treatment and magnetic field treatment are adopted, and through reasonable selection of technological parameters of the auxiliary means, the mutual cooperation of the ultrasonic treatment, the microwave treatment and the magnetic field treatment can improve the preparation efficiency and the yield of the nanocellulose, and the preparation of the nanocellulose can be realized in a green efficient manner by combining the method with mechanical grinding, so that the consumption of a dispersing agent is effectively reduced, the cost is saved, and the environmental pollution is reduced.
Detailed Description
In order to better understand the technical solution of the present invention, the following describes the product of the present invention in further detail with reference to examples.
Example 1
A green efficient preparation method of nanocellulose comprises the following steps:
step S1, pretreatment of cellulose raw materials: cutting cellulose raw material into powder by a dry method at high frequency;
step S2, preparation of cellulose dispersion liquid: adding the cellulose powder prepared in the step S1 into a dispersing agent, and uniformly dispersing to prepare cellulose dispersion liquid;
step S3, mechanical grinding: grinding the cellulose dispersion liquid prepared in the step S2 in a P7 miniature planetary high-energy ball mill for 1h;
step S4, centrifugal separation: and (3) separating the dispersion liquid obtained through the treatment in the step (S3) by adopting a centrifugal machine to obtain supernatant containing cellulose nanocrystals, and then carrying out vacuum filtration and defoaming on the supernatant to prepare the cellulose nanocrystals.
The powder in step S1 has a width in the range of 8 μm and a length in the range of 20. Mu.m; the cellulose raw material in the step S1 is bamboo cellulose.
The dispersant in the step S2 is water; the mass percentage concentration of the cellulose dispersion liquid is 0.5 weight percent.
In the step S3, the grinding is intermittent grinding, and each grinding time is 15 minutes and 10 minutes; the mechanical grinding is preceded by ultrasonic treatment, microwave treatment and magnetic field treatment; the ultrasonic treatment frequency is 50kHz, the power range is 400W, and the treatment time is 15min; the frequency of the microwave treatment is 2.2GHz, the power range is 600W, and the treatment time is 5min; the magnetic field strength of the magnetic field treatment is 7500Gs, and the treatment time is 10min.
The centrifuge in step S4 was controlled to have a rotational speed of 3500rpm during centrifugation.
The nanocellulose prepared by the nanocellulose green efficient preparation method.
Example 2
A green efficient preparation method of nanocellulose comprises the following steps:
step S1, pretreatment of cellulose raw materials: cutting cellulose raw material into powder by a dry method at high frequency;
step S2, preparation of cellulose dispersion liquid: adding the cellulose powder prepared in the step S1 into a dispersing agent, and uniformly dispersing to prepare cellulose dispersion liquid;
step S3, mechanical grinding: grinding the cellulose dispersion liquid prepared in the step S2 in a P7 miniature planetary high-energy ball mill for 1h;
step S4, centrifugal separation: and (3) separating the dispersion liquid obtained through the treatment in the step (S3) by adopting a centrifugal machine to obtain supernatant containing cellulose nanocrystals, and then carrying out vacuum filtration and defoaming on the supernatant to prepare the cellulose nanocrystals.
The powder in step S1 has a width in the range of 12 μm and a length in the range of 30. Mu.m; the cellulose raw material is flax cellulose.
The dispersant in the step S2 is ethanol; the mass percentage concentration of the cellulose dispersion liquid is 2wt%.
In the step S3, the grinding is intermittent grinding, and each grinding time is 15 minutes and 10 minutes; the mechanical grinding is preceded by ultrasonic treatment, microwave treatment and magnetic field treatment; the ultrasonic treatment frequency is 60kHz, the power range is 500W, and the treatment time is 20min; the frequency of the microwave treatment is 2.3GHz, the power range is 800W, and the treatment time is 10min; the magnetic field strength of the magnetic field treatment is 9500Gs, and the treatment time is 15min.
During the centrifugation of the centrifuge in step S4, the rotational speed was controlled to 4500rpm.
The nanocellulose prepared by the nanocellulose green efficient preparation method.
Example 3
A green efficient preparation method of nanocellulose comprises the following steps:
step S1, pretreatment of cellulose raw materials: cutting cellulose raw material into powder by a dry method at high frequency;
step S2, preparation of cellulose dispersion liquid: adding the cellulose powder prepared in the step S1 into a dispersing agent, and uniformly dispersing to prepare cellulose dispersion liquid;
step S3, mechanical grinding: grinding the cellulose dispersion liquid prepared in the step S2 in a P7 miniature planetary high-energy ball mill for 1.5h;
step S4, centrifugal separation: and (3) separating the dispersion liquid obtained through the treatment in the step (S3) by adopting a centrifugal machine to obtain supernatant containing cellulose nanocrystals, and then carrying out vacuum filtration and defoaming on the supernatant to prepare the cellulose nanocrystals.
The powder in step S1 has a width in the range of 14 μm and a length in the range of 35. Mu.m; the cellulose raw material is alginate cellulose; the dispersant in the step S2 is water; the mass percentage concentration of the cellulose dispersion liquid is 4wt%.
In the step S3, the grinding is intermittent grinding, and each grinding time is 15 minutes and 10 minutes; the mechanical grinding is preceded by ultrasonic treatment, microwave treatment and magnetic field treatment; the ultrasonic treatment frequency is 65kHz, the power range is 600W, and the treatment time is 25min; the frequency of the microwave treatment is 2.4GHz, the power range is 1000W, and the treatment time is 14min; the magnetic field strength of the magnetic field treatment is 13500Gs, and the treatment time is 19min.
The centrifuge in step S4 was controlled to have a rotation speed of 6000rpm during centrifugation.
The nanocellulose prepared by the nanocellulose green efficient preparation method.
Example 4
A green efficient preparation method of nanocellulose comprises the following steps:
step S1, pretreatment of cellulose raw materials: cutting cellulose raw material into powder by a dry method at high frequency;
step S2, preparation of cellulose dispersion liquid: adding the cellulose powder prepared in the step S1 into a dispersing agent, and uniformly dispersing to prepare cellulose dispersion liquid;
step S3, mechanical grinding: grinding the cellulose dispersion liquid prepared in the step S2 in a P7 miniature planetary high-energy ball mill for 2 hours;
step S4, centrifugal separation: and (3) separating the dispersion liquid obtained through the treatment in the step (S3) by adopting a centrifugal machine to obtain supernatant containing cellulose nanocrystals, and then carrying out vacuum filtration and defoaming on the supernatant to prepare the cellulose nanocrystals.
The powder in step S1 has a width in the range of 18 μm and a length in the range of 45. Mu.m; the cellulose raw material in the step S1 is microcrystalline cellulose which is processed manually.
The dispersing agent in the step S2 is a mixture formed by mixing water and ethanol according to a mass ratio of 3:5; the mass percentage concentration of the cellulose dispersion liquid is 5wt%; in the step S3, the grinding is intermittent grinding, and each grinding time is 15 minutes and 10 minutes; the step S3 is characterized by further comprising ultrasonic treatment, microwave treatment and magnetic field treatment before mechanical grinding; the ultrasonic treatment frequency is 75kHz, the power range is 750W, and the treatment time is 30min; the frequency of the microwave treatment is 2.4GHz, the power range is 1200W, and the treatment time is 17min; the magnetic field strength of the magnetic field treatment is 15500Gs, and the treatment time is 23min; the centrifuge in step S4 was controlled to rotate at 7000rpm during centrifugation.
The nanocellulose prepared by the nanocellulose green efficient preparation method.
Example 5
A green efficient preparation method of nanocellulose comprises the following steps:
step S1, pretreatment of cellulose raw materials: cutting cellulose raw material into powder by a dry method at high frequency;
step S2, preparation of cellulose dispersion liquid: adding the cellulose powder prepared in the step S1 into a dispersing agent, and uniformly dispersing to prepare cellulose dispersion liquid;
step S3, mechanical grinding: grinding the cellulose dispersion liquid prepared in the step S2 in a P7 miniature planetary high-energy ball mill for 2 hours;
step S4, centrifugal separation: and (3) separating the dispersion liquid obtained through the treatment in the step (S3) by adopting a centrifugal machine to obtain supernatant containing cellulose nanocrystals, and then carrying out vacuum filtration and defoaming on the supernatant to prepare the cellulose nanocrystals.
The powder in step S1 has a width in the range of 20 μm and a length in the range of 50. Mu.m; the cellulose raw material in the step S1 is bamboo cellulose.
The dispersant in the step S2 is water; the mass percentage concentration of the cellulose dispersion liquid is 5.5wt%; in the step S3, the grinding is intermittent grinding, and each grinding time is 15 minutes and 10 minutes; the step S3 is characterized by further comprising ultrasonic treatment, microwave treatment and magnetic field treatment before mechanical grinding; the ultrasonic treatment frequency is 80kHz, the power range is 800W, and the treatment time is 35min; the frequency of the microwave treatment is 2.5GHz, the power range is 1300W, and the treatment time is 20min; the magnetic field strength of the magnetic field treatment is 16500Gs, and the treatment time is 25min; the centrifuge in step S4 was controlled to rotate at 7500rpm during centrifugation.
The nanocellulose prepared by the nanocellulose green efficient preparation method.
Comparative example 1
A green efficient preparation method of nanocellulose, which is substantially the same as example 1, except that there is no ultrasonic treatment and no magnetic field treatment.
Comparative example 2
A green efficient preparation method of nanocellulose, which is substantially the same as example 1, except that no microwave treatment is performed.
Meanwhile, in order to evaluate the specific technical effects of the green efficient preparation method of the nanocellulose, statistical calculation is performed on the yield and the relative crystallinity of the nanocellulose prepared by the preparation methods of each example, and the results are shown in table 1.
TABLE 1
| Project | Yield (%) | Relative crystallinity (%) |
| Example 1 | 88.5 | 80.79 |
| Example 2 | 89.3 | 80.98 |
| Example 3 | 89.9 | 81.53 |
| Example 4 | 90.9 | 81.92 |
| Example 5 | 91.4 | 82.27 |
| Comparative example 1 | 85.3 | 78.88 |
| Comparative example 2 | 84.6 | 77.95 |
As can be seen from Table 1, the green efficient preparation method of nanocellulose disclosed in the examples of the present invention has better yield and higher relative crystallinity than the comparative examples, and the ultrasonic treatment, the magnetic field treatment and the microwave treatment are beneficial to improving the above properties.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention in any way; those of ordinary skill in the art will readily implement the invention as described above; however, those skilled in the art will appreciate that many modifications, adaptations, and variations of the present invention are possible in light of the above teachings without departing from the scope of the invention; meanwhile, any equivalent changes, modifications and evolution of the above embodiments according to the essential technology of the present invention still fall within the scope of the present invention.
Claims (10)
1. The green efficient preparation method of the nanocellulose is characterized by comprising the following steps of:
step S1, pretreatment of cellulose raw materials: cutting cellulose raw material into powder by a dry method at high frequency;
step S2, preparation of cellulose dispersion liquid: adding the cellulose powder prepared in the step S1 into a dispersing agent, and uniformly dispersing to prepare cellulose dispersion liquid;
step S3, mechanical grinding: grinding the cellulose dispersion liquid prepared in the step S2 in a P7 miniature planetary high-energy ball mill for 1-2h;
step S4, centrifugal separation: and (3) separating the dispersion liquid obtained through the treatment in the step (S3) by adopting a centrifugal machine to obtain supernatant containing cellulose nanocrystals, and then carrying out vacuum filtration and defoaming on the supernatant to prepare the cellulose nanocrystals.
2. The method for green and efficient production of nanocellulose as claimed in claim 1 wherein said powder in step S1 has a width ranging from 8 to 20 μm and a length ranging from 20 to 50 μm.
3. The method for preparing nano-cellulose according to claim 1, wherein the cellulose raw material in step S1 is any one of bamboo cellulose, flax cellulose, seaweed cellulose and artificially treated microcrystalline cellulose.
4. The method for preparing nanocellulose in green and efficient manner as claimed in claim 1, wherein the dispersant in step S2 is at least one of water and ethanol.
5. The method for green and efficient preparation of nanocellulose as claimed in claim 1 wherein the mass percentage concentration of said cellulose dispersion in step S2 is 0.5wt% to 5.5wt%.
6. The method for green and efficient preparation of nanocellulose as claimed in claim 1 wherein the grinding in step S3 is batch grinding, each 15min batch for 10min.
7. The method for green and efficient preparation of nanocellulose as claimed in claim 1 wherein said mechanical grinding in step S3 further comprises ultrasonic treatment, microwave treatment and magnetic field treatment.
8. The efficient green nanocellulose preparation method of claim 7, wherein said ultrasonic treatment frequency is 50-80kHz, power range is 400-800W, and treatment time is 15-35min; the frequency of the microwave treatment is 2.2-2.5GHz, the power range is 600-1300W, and the treatment time is 5-20min; the magnetic field strength of the magnetic field treatment is 7500-16500Gs, and the treatment time is 10-25min.
9. The method for preparing nanocellulose in green and efficient manner as claimed in claim 1, wherein the rotational speed of the centrifuge in step S4 is controlled to 3500-7500 rpm during centrifugation.
10. A nanocellulose prepared by the green efficient nanocellulose preparation method of any one of claims 1-9.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584059A (en) * | 2012-01-21 | 2012-07-18 | 东北林业大学 | Preparation method of rapid dispersion powder for nano-crystalline cellulose |
| CN106883301A (en) * | 2017-02-22 | 2017-06-23 | 中国科学院理化技术研究所 | Method for simultaneously preparing cellulose nanocrystals and cellulose nanofibers |
| CN116084199A (en) * | 2023-03-09 | 2023-05-09 | 浙江科技学院 | Method for preparing nanofibrillar cellulose by ultrasonic swelling auxiliary mechanical grinding |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584059A (en) * | 2012-01-21 | 2012-07-18 | 东北林业大学 | Preparation method of rapid dispersion powder for nano-crystalline cellulose |
| CN106883301A (en) * | 2017-02-22 | 2017-06-23 | 中国科学院理化技术研究所 | Method for simultaneously preparing cellulose nanocrystals and cellulose nanofibers |
| CN116084199A (en) * | 2023-03-09 | 2023-05-09 | 浙江科技学院 | Method for preparing nanofibrillar cellulose by ultrasonic swelling auxiliary mechanical grinding |
Non-Patent Citations (1)
| Title |
|---|
| 裴继诚主编: "《植物纤维化学》", vol. 5, 31 May 2020, 中国轻工业出版社, pages: 215 * |
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