CN106119315A - A kind of green method of functional modification nano-cellulose - Google Patents
A kind of green method of functional modification nano-cellulose Download PDFInfo
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Abstract
The invention discloses the green method of a kind of functional modification nano-cellulose.The cellulosic material of drying is first joined in ionic liquid by the method, heated at constant temperature stirs, the solution obtained is down to room temperature, add lipase, fatty acid methyl ester, ionic liquid, lipase consumption is the 2% ~ 50% of cellulose quality, fatty acid methyl ester is 1:1 ~ 13:1 with the mol ratio of cellulose, reacts 1 ~ 8h at 20 DEG C ~ 80 DEG C.Reaction terminates, and adds dehydrated alcohol and carries out washing, being centrifuged, remove supernatant after solution cools down, and the precipitate obtained is dried 12 ~ 48h at 40 ~ 80 DEG C, i.e. obtains the functional modification nano-cellulose of the present invention.The present invention has the advantages such as the most efficient, reproducible, technical process and agents useful for same environmental protection, is with a wide range of applications in fields such as membrane material, medicinal slow release agent, optical materials.
Description
Technical field
The present invention relates to the field of production of nano-cellulose, be specifically related to a kind of functional modification nano-cellulose
Green method.
Background technology
Nano-cellulose is that native cellulose molecule is softened, activation and enzyme action etc. process obtain for attenuated fibers element,
Because it has high-crystallinity, the high grade of transparency, high Young's modulus, the feature such as renewable, aobvious in high-performance composite materials field at present
The biggest application prospect is shown.But, nano-cellulose specific surface area is big, and great amount of hydroxy group is contained on surface, between cellulose grain
Being easy to the interaction by hydrogen bond reunite, the very difficult physical method of cellulose grain after reunion is scatter.
Therefore, prepare functional modification nano-cellulose, reduce hydrophilic and the polarity of nano-cellulose, improve its interface compatibility,
It it is the important means of the cellulose enhancing composite that processability is excellent.
At present, the method such as the preparation method of nano-cellulose predominantly organic tool method, chemical method, bioanalysis.Pass through Mechanical Method
Preparing nano-cellulose, it is not necessary to chemical reagent, effect on environment is little.But use nano-cellulose particle diameter distribution prepared by Mechanical Method
Width, and Preparation equipment is special, energy expenditure is high.While chemical method prepares nano-cellulose, also can to its modifying surface,
Thus give the new function of nano micro crystal cellulose and characteristic.Chemical method generally comprises acid-hydrolysis method, enzymatic isolation method etc., to equipment
Require relatively stricter, and have greater environmental impacts.It is low energy consumption, pollution-free that bioanalysis prepares the great advantage of nano-cellulose,
But it is low that bioanalysis prepares nano-cellulose process length complicated, time-consuming, cost height, price, yield.
It addition, the main method that nano-cellulose surface modification is commonly used has alkali process, oxidation processes, glycerol polymerization, Re Chu
Reason etc..All there are a certain degree of shortcomings and deficiencies in these methods, strict to equipment requirements, and technological requirement is high, easy damaged fiber,
And these method of modifying, the overwhelming majority to bark at muttering etc. at toluene, tetrahydrochysene and to carry out in the bigger organic solvent of toxicity, and reaction condition is severe
Carving, reaction scheme is complicated, and industrializing implementation cost is high.Therefore, explore environmental protection, new and effective nano-cellulose surface is dredged
Aquation method of modifying, is the important means of the cellulose enhancing composite that processability is excellent.
Green Chemistry has become as the forward position of current chemical science development, is the important directions of chemical developer in this century.Make
For a kind of novel reaction medium, ionic liquid is described as one of optimal reaction medium in 21 century cleaning green industry.This
Invent the angle from Green Chemistry, seek a kind of method preparing functional modification nano-cellulose of environmental protection.Utilize from
Sub-liquid tasteless, pollution-free, nonflammable, easily separate with product, easily reclaim, can repeated multiple times recycling and easy to use etc.
Advantage, the use that efficiently avoid conventional organic solvents is caused serious environment, health, safety and equipment corrosion etc. to ask
Topic.By research enzymatic clarification of functional modification nano-cellulose in ionic liquid, propose a green new technology, open up
The application in cellulose esters synthesizes of the exhibition living things catalysis, excellent as industrial chemicals processability at replacement fossil resource for cellulose
Good industrial chemical aspect provides the biggest development potentiality.
Summary of the invention
Present invention aims to problem present in current modifying nanometer cellulose process, it is provided that a kind of to environment
Close friend, reaction condition gentleness, convenient product separation, equipment needed thereby and simple to operate, lipase in green solvent ionic liquid
The method catalyzing and synthesizing functional modification nano-cellulose.
The purpose of the present invention is achieved through the following technical solutions.
The preparation method of a kind of functional modification nano-cellulose, comprises the steps:
(1) cellulosic material is dried；
(2) with sulfur hydrogen acidic ionic liquids, step (1) gained cellulose being made into cellulose mass percent concentration is 5 ~ 20%
Mixture, stirs 1 ~ 5h in 70 ~ 100 DEG C of constant temperature；
(3) solution of step (2) gained is down to room temperature, adds lipase, ionic liquid and fatty acid methyl ester, in 20 DEG C ~ 80
DEG C reaction 1 ~ 8h；Described ionic liquid is the one in Tetrafluoroboric acid class and hexafluorophosphoric acid class ionic liquid, hydrogen sulfate salt from
Sub-liquid is 3:5 with the mass ratio of fluorate ionic liquid；Described lipase consumption is the 2% ~ 50% of cellulosic material quality, institute
The mol ratio stating fatty acid methyl ester and cellulosic material is 1:1 ~ 13:1；
(4) solution that step (3) obtains is cooled to room temperature, adds dehydrated alcohol and carry out washing, being centrifuged, remove supernatant, will
The drying precipitate obtained, i.e. obtains functional modification nano-cellulose.
Further, step (1) described cellulosic material be microcrystalline Cellulose, wood pulp cellulose, cotton fiber, straw pulp fiber,
Paper pulp raw material etc..
Further, the temperature of step (1) described drying is 40 ~ 90 DEG C.
Further, step (2) described sulfur hydrogen salt class ionic liquid is 1-butyl-3-Methylimidazole. sulfur hydrogen salt
([BMIM] HSO4), 1-ethyl-3-methylimidazole sulfur hydrogen salt, 1-propyl group-3-Methylimidazole. sulfur hydrogen salt, 1-pi-allyl-3-
Methylimidazole. sulfur hydrogen salt or 1-hexyl-3-Methylimidazole. sulfur hydrogen salt.
Further, step (2) described sulfur hydrogen salt class ionic liquid is 1-butyl-3-Methylimidazole. sulfur hydrogen salt
([BMIM] HSO4).
Further, the sulfur hydrogen salt class ionic liquid in step (2) with the mass ratio of the ionic liquid in step (3) is
3:5。
Further, step (3) described ionic liquid is 1-butyl-3-methyl imidazolium tetrafluoroborate ([BMIM] BF4).
Further, step (3) described fatty acid methyl ester is methyl laurate, methyl hexadecanoate or methyl stearate.
Further, step (3) described fatty acid methyl ester is methyl laurate.
Further, step (3) described lipase derives from Candida rugosa(Candida cylindracea), Porcine
Pancreatic(Pancreas Sus domestica gland), Thermomyces lanuginosus(Thermomyces lanuginosus), Candida
Antarctica B(antarctic candida B) or Pseudomonas(bacillus pyocyaneus).
Further, step (3) described lipase derives from Candida rugosa.
Further, step (4) described washing is without ionic liquid and fatty acid with absolute ethanol washing to precipitate
The impurity such as methyl ester.
Further, step (4) described vacuum drying be the precipitate obtained is vacuum dried at 40 ~ 80 DEG C 12 ~
48h。
The present invention compared with prior art, has the advantage that and beneficial effect:
1, the present invention uses ionic liquid to replace conventional organic solvents as solvent, this solvent safety, nontoxic, harmless, will not be right
Environment.
2, the ionic liquid 1-butyl-3-methyl imidazolium sulfur hydrogen salt that the present invention uses at high temperature can selective destruction fibre
The amorphous region of dimension element, effective decomposition of cellulose becomes nano-cellulose.
3, the lipase that the present invention uses is in ionic liquid 1-butyl-3-methyl imidazolium tetrafluoroborate, can be preferably
Keeping its molecular structure, the required reaction condition of its esterification is gentle, and catalytic efficiency is high.
4, process route of the present invention is simple, green, safety, and obtained product can be applicable to food, medicine
Higher field is required Deng to Product Safety.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of functional modification nano-cellulose in microcrystalline Cellulose and embodiment.
Fig. 2 is the transmission electron microscope picture of functional modification nano-cellulose in microcrystalline Cellulose and embodiment.
Detailed description of the invention
For being best understood from the present invention, below in conjunction with embodiment the present invention done and describe in detail further, but the present invention
Claimed scope is not limited to the scope that embodiment represents.
Embodiment 1
The first step: microcrystalline Cellulose 0.5g is dried at 50 DEG C 48h；
Second step: with [BMIM] HSO4First step gained cellulose is made into the mixing that cellulose mass percent concentration is 5%
Thing, stirs 1h in 70 DEG C of constant temperature；
3rd step: second step gained solution is down to room temperature, adds lipase CRL, ionic liquid [BMIM] BF4([BMIM]
HSO4/ [BMIM]BF4Mass ratio is 3:5) and methyl laurate, lipase CRL consumption is the 20% of microcrystalline Cellulose quality, the moon
Acid methylester is 3:1 with the mol ratio of microcrystalline Cellulose, reacts 3h in 50 DEG C；；
4th step: the solution obtained by the 3rd step is cooled to room temperature, adds dehydrated alcohol and carries out washing, being centrifuged, remove supernatant
Liquid, the precipitate obtained is dried 24h at 60 DEG C, i.e. obtains functional modification nano-cellulose.Detect through acid-base titrations, this
The substitution value of embodiment gained functional modification nano-cellulose is 0.092.
Acid-base titrations is the universal method that esterification cellulose ester substitution value measures, and can record its molecule by infrared spectrometry
Change in structure, mainly shows as at 1730 ~ 1750cm-1There is a new absworption peak in left and right, and the appearance at this peak proves fibre
Dimension element molecule generation esterification, defines fatty acid cellulose ester.
Fatty acid cellulose ester substitution value assay method: the concrete method of testing of acid-base titrations is for accurately weighing sample
0.2g, is placed in conical flask, in NaOH and the 50ml distilled water of the 0.2mol/ L being dissolved in 20ml, stirs 30min at 75 DEG C.
Transfer the solution in the volumetric flask of 100mL, add distilled water to mark line.This solution of 25mL is transferred in 50mL conical flask, uses
The NaOH of the HCl titer overtitration of 0.05mol/ L.And use phenolphthalein indicator.Titrate in triplicate, hydrochloric acid volume
Meansigma methods V is used for calculating.Doing blank assay, record titration consumes volume V simultaneously0。
DS=162n/(0.2-M’*n)
N=162 * 4*c*(V0-V)
Wherein: c is hydrochloric acid standard solution concentration (mol/L)；V0It is respectively blank with V and consumes volume and sample titration consumer
Long-pending, M ' is the net increase of the quality in each carboxyl group that an AGU is replaced.
Embodiment 2
The first step: microcrystalline Cellulose 0.5g is dried at 50 DEG C 48h；
Second step: with [EMIM] HSO4First step gained cellulose is made into the mixing that cellulose mass percent concentration is 5%
Thing, stirs 2h in 100 DEG C of constant temperature；
3rd step: second step gained solution is down to room temperature, adds lipase CRL, ionic liquid [BMIM] BF4([BMIM]
HSO4/ [BMIM]BF4Mass ratio is 3:5) and methyl laurate, lipase CRL consumption is the 15% of microcrystalline Cellulose quality, the moon
Acid methylester is 3:1 with the mol ratio of microcrystalline Cellulose, reacts 3h in 60 DEG C；；
4th step: the solution obtained by the 3rd step is cooled to room temperature, adds dehydrated alcohol and carries out washing, being centrifuged, remove supernatant
Liquid, the precipitate obtained is dried 24h at 60 DEG C, i.e. obtains functional modification nano-cellulose.Detect through acid-base titrations, this
The substitution value of embodiment gained functional modification nano-cellulose is 0.113.
The infrared spectrogram of the functional modification nano-cellulose that the present embodiment prepares is as shown in curve b in Figure 1.
Embodiment 3
The first step: microcrystalline Cellulose 0.5g is dried at 80 DEG C 48h；
Second step: with [BMIM] HSO4First step gained cellulose is made into the mixing that cellulose mass percent concentration is 10%
Thing, stirs 3h in 80 DEG C of constant temperature；
3rd step: second step gained solution is down to room temperature, adds lipase CRL, ionic liquid [BMIM] BF4([BMIM]
HSO4/ [BMIM]BF4Mass ratio is 3:5) and methyl laurate, lipase CRL consumption is the 15% of microcrystalline Cellulose quality, the moon
Acid methylester is 13:1 with the mol ratio of microcrystalline Cellulose, reacts 5h in 60 DEG C；；
4th step: the solution obtained by the 3rd step is cooled to room temperature, adds dehydrated alcohol and carries out washing, being centrifuged, remove supernatant
Liquid, the precipitate obtained is dried 24h at 60 DEG C, i.e. obtains functional modification nano-cellulose.Detect through acid-base titrations, this
The substitution value of embodiment gained functional modification nano-cellulose is 0.158.
Embodiment 4
The first step: microcrystalline Cellulose 0.5g is dried at 70 DEG C 48h；
Second step: with [BMIM] HSO4First step gained cellulose is made into the mixing that cellulose mass percent concentration is 15%
Thing, stirs 2h in 100 DEG C of constant temperature；
3rd step: second step gained solution is down to room temperature, adds lipase CRL, ionic liquid [BMIM] BF4([BMIM]
HSO4/ [BMIM]BF4Mass ratio is 3:5) and methyl laurate, lipase CRL consumption is the 15% of microcrystalline Cellulose quality, the moon
Acid methylester is 6:1 with the mol ratio of microcrystalline Cellulose, reacts 1h in 80 DEG C；；
4th step: the solution obtained by the 3rd step is cooled to room temperature, adds dehydrated alcohol and carries out washing, being centrifuged, remove supernatant
Liquid, the precipitate obtained is dried 24h at 60 DEG C, i.e. obtains functional modification nano-cellulose.Detect through acid-base titrations, this
The substitution value of embodiment gained functional modification nano-cellulose is 0.095.
Embodiment 5
The first step: microcrystalline Cellulose 0.5g is dried at 50 DEG C 48h；
Second step: with [BMIM] HSO4First step gained cellulose is made into the mixing that cellulose mass percent concentration is 20%
Thing, stirs 3h in 90 DEG C of constant temperature；
3rd step: second step gained solution is down to room temperature, adds lipase CRL, ionic liquid [BMIM] BF4([BMIM]
HSO4/ [BMIM]BF4Mass ratio is 3:5) and methyl laurate, lipase CRL consumption is the 20% of microcrystalline Cellulose quality, the moon
Acid methylester is 5:1 with the mol ratio of microcrystalline Cellulose, reacts 2h in 60 DEG C；；
4th step: the solution obtained by the 3rd step is cooled to room temperature, adds dehydrated alcohol and carries out washing, being centrifuged, remove supernatant
Liquid, the precipitate obtained is dried 24h at 60 DEG C, i.e. obtains functional modification nano-cellulose.Detect through acid-base titrations, this
The substitution value of embodiment gained functional modification nano-cellulose is 0.101.
Embodiment 6
The first step: microcrystalline Cellulose 0.5g is dried at 40 DEG C 48h；
Second step: with [BMIM] HSO4First step gained cellulose is made into the mixing that cellulose mass percent concentration is 10%
Thing, stirs 5h in 70 DEG C of constant temperature；
3rd step: second step gained solution is down to room temperature, adds lipase CRL, ionic liquid [BMIM] BF4([BMIM]
HSO4/ [BMIM]BF4Mass ratio is 3:5) and methyl laurate, lipase CRL consumption is the 10% of microcrystalline Cellulose quality, the moon
Acid methylester is 9:1 with the mol ratio of microcrystalline Cellulose, reacts 4h in 70 DEG C；；
4th step: the solution obtained by the 3rd step is cooled to room temperature, adds dehydrated alcohol and carries out washing, being centrifuged, remove supernatant
Liquid, the precipitate obtained is dried 24h at 60 DEG C, i.e. obtains functional modification nano-cellulose.Detect through acid-base titrations, this
The substitution value of embodiment gained functional modification nano-cellulose is 0.142.
Embodiment 7
The first step: microcrystalline Cellulose 0.5g is dried at 80 DEG C 48h；
Second step: with [BMIM] HSO4First step gained cellulose is made into the mixing that cellulose mass percent concentration is 10%
Thing, stirs 4h in 70 DEG C of constant temperature；
3rd step: second step gained solution is down to room temperature, adds lipase CRL, ionic liquid [BMIM] BF4([BMIM]
HSO4/ [BMIM]BF4Mass ratio is 3:5) and methyl laurate, lipase CRL consumption is the 50% of microcrystalline Cellulose quality, the moon
Acid methylester is 8:1 with the mol ratio of microcrystalline Cellulose, reacts 6h in 70 DEG C；；
4th step: the solution obtained by the 3rd step is cooled to room temperature, adds dehydrated alcohol and carries out washing, being centrifuged, remove supernatant
Liquid, the precipitate obtained is dried 24h at 60 DEG C, i.e. obtains functional modification nano-cellulose.Detect through acid-base titrations, this
The substitution value of embodiment gained functional modification nano-cellulose is 0.151.
The present embodiment prepares the infrared spectrogram of long chain fatty acid cellulose element ester as shown in curve c in Figure 1.
Embodiment 8
The first step: microcrystalline Cellulose 0.5g is dried at 40 DEG C 48h；
Second step: with [BMIM] HSO4First step gained cellulose is made into the mixing that cellulose mass percent concentration is 5%
Thing, stirs 5h in 80 DEG C of constant temperature；
3rd step: second step gained solution is down to room temperature, adds lipase CRL, ionic liquid [BMIM] BF4([BMIM]
HSO4/ [BMIM]BF4Mass ratio is 3:5) and methyl laurate, lipase CRL consumption is the 2% of microcrystalline Cellulose quality, Laurel
Acid methyl ester is 8:1 with the mol ratio of microcrystalline Cellulose, reacts 8h in 80 DEG C；；
4th step: the solution obtained by the 3rd step is cooled to room temperature, adds dehydrated alcohol and carries out washing, being centrifuged, remove supernatant
Liquid, the precipitate obtained is dried 24h at 60 DEG C, i.e. obtains functional modification nano-cellulose.Detect through acid-base titrations, this
The substitution value of embodiment gained functional modification nano-cellulose is 0.015.
Embodiment 9
The first step: microcrystalline Cellulose 0.5g is dried at 40 DEG C 48h；
Second step: with [BMIM] HSO4First step gained cellulose is made into the mixing that cellulose mass percent concentration is 20%
Thing, stirs 3h in 70 DEG C of constant temperature；
3rd step: second step gained solution is down to room temperature, adds lipase CRL, ionic liquid [BMIM] BF4([BMIM]
HSO4/ [BMIM]BF4Mass ratio is 3:5) and methyl laurate, lipase CRL consumption is the 30% of microcrystalline Cellulose quality, the moon
Acid methylester is 1:1 with the mol ratio of microcrystalline Cellulose, reacts 6h in 20 DEG C；；
4th step: the solution obtained by the 3rd step is cooled to room temperature, adds dehydrated alcohol and carries out washing, being centrifuged, remove supernatant
Liquid, the precipitate obtained is dried 24h at 60 DEG C, i.e. obtains functional modification nano-cellulose.Detect through acid-base titrations, this
The substitution value of embodiment gained functional modification nano-cellulose is 0.022.
Table 1 is the result of embodiment 1-9 functional modification nano-cellulose substitution value.
Table 1
| Sample | Concentration of substrate | Treatment temperature | The process time | Lipase consumption | Fatty acid methyl ester consumption | Reaction temperature | Response time | Substitution value |
| Embodiment 1 | 5% | 70℃ | 1h | 20% | 3:1 | 50℃ | 3h | 0.092 |
| Embodiment 2 | 5% | 100℃ | 2h | 15% | 3:1 | 60℃ | 3h | 0.113 |
| Embodiment 3 | 10% | 80℃ | 3h | 15% | 13:1 | 60℃ | 5h | 0.158 |
| Embodiment 4 | 15% | 100℃ | 2h | 15% | 6:1 | 80℃ | 1h | 0.095 |
| Embodiment 5 | 20% | 90℃ | 3h | 20% | 5:1 | 60℃ | 2h | 0.101 |
| Embodiment 6 | 10% | 70℃ | 5h | 10% | 9:1 | 70℃ | 4h | 0.142 |
| Embodiment 7 | 10% | 70℃ | 4h | 50% | 8:1 | 70℃ | 6h | 0.151 |
| Embodiment 8 | 5% | 80℃ | 5h | 2% | 8:1 | 80℃ | 8h | 0.015 |
| Embodiment 9 | 20% | 70℃ | 3h | 30% | 1:1 | 20℃ | 6h | 0.022 |
The infrared spectrogram of different degree of substitution functional modification nano-cellulose is as shown in Figure 1.In figure, curve a is former microcrystalline cellulose
The infrared spectrogram of element, curve b is the infrared spectrum of the functional modification nano-cellulose (DS is 0.113) that embodiment 2 prepares
Figure, curve c is the infrared spectrogram of the functional modification nano-cellulose (DS is 0.151) that embodiment 7 prepares.Obtained merit
Energyization modification nano-cellulose curve is compared with former microcrystalline Cellulose curve, at 1740cm-1Place occurs in that former microcrystalline Cellulose does not has
Some ester group absworption peaks, show cellulosic molecule generation esterification, define cellulose esters, and along with the increasing of substitution value
Adding, ester group absorption peak strength strengthens.
The scanning electron microscope (SEM) photograph of functional modification nano-cellulose is as shown in Figure 2.Obtained functional modification nanofiber
The diameter about 20 ~ 80nm of element.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not limited by above-described embodiment
System, the modification made, changes, substitutes, combines, simplifies, all under other any spirit without departing from the present invention and principle
Should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (10)
1. the green method of a functional modification nano-cellulose, it is characterised in that comprise the steps:
(1) cellulosic material is dried；
(2) with sulfur hydrogen salt class ionic liquid, step (1) gained cellulose being made into cellulose mass percent concentration is 5 ~ 20%
Mixture, stir 1 ~ 5h in 70 ~ 100 DEG C of constant temperature；
(3) solution of step (2) gained is down to room temperature, adds lipase, ionic liquid and fatty acid methyl ester, in 20 DEG C ~ 80
DEG C reaction 1 ~ 8h；Described ionic liquid is more than one in Tetrafluoroboric acid salt and hexafluorophosphoric acid salt ionic liquid, ion
The solution of step (2) gained is made into the mixture that ionic liquid mass content is 3 ~ 15% by liquid；Described lipase consumption is fine
The 2% ~ 50% of dimension element raw materials quality, described fatty acid methyl ester is 1:1 ~ 13:1 with the mol ratio of cellulosic material；
(4) solution that step (3) obtains is cooled to room temperature, adds dehydrated alcohol and carry out washing, being centrifuged, remove supernatant, will
The precipitate vacuum drying obtained, i.e. obtains functional modification nano-cellulose.
The green method of a kind of functional modification nano-cellulose the most according to claim 1, it is characterised in that: step
(1) described cellulosic material is microcrystalline Cellulose, wood pulp cellulose, cotton fiber, straw pulp fiber or paper pulp.
The green method of a kind of functional modification nano-cellulose the most according to claim 1, it is characterised in that: step
(1) temperature of described drying is 40 ~ 90 DEG C.
The green method of a kind of functional modification nano-cellulose the most according to claim 1, it is characterised in that: step
(2) described sulfur hydrogen salt class ionic liquid is 1-butyl-3-Methylimidazole. sulfur hydrogen salt, 1-ethyl-3-methylimidazole sulfur hydracid
Salt, 1-propyl group-3-Methylimidazole. sulfur hydrogen salt, 1-pi-allyl-3-Methylimidazole. sulfur hydrogen salt or 1-hexyl-3-Methylimidazole. sulfur
Hydrohalogenic acid salt.
The green method of a kind of functional modification nano-cellulose the most according to claim 1, it is characterised in that: step
(3) described ionic liquid is 1-butyl-3-methyl imidazolium tetrafluoroborate or 1-butyl-3-Methylimidazole. hexafluorophosphate.
The green method of a kind of functional modification nano-cellulose the most according to claim 1, it is characterised in that: step
(3) described fatty acid methyl ester is methyl laurate, methyl hexadecanoate or methyl stearate.
The green method of a kind of functional modification nano-cellulose the most according to claim 1, it is characterised in that: step
(3) described lipase derive from Candida rugosa, Porcine pancreatic, Thermomyces lanuginosus,
Candida antarctica B or Pseudomonas.
The green method of a kind of functional modification nano-cellulose the most according to claim 1, it is characterised in that: step
(4) described washing is without ionic liquid and fatty acid methyl ester with absolute ethanol washing to precipitate.
The green method of a kind of functional modification nano-cellulose the most according to claim 1, it is characterised in that: step
(4) described vacuum drying is that the precipitate obtained is dried at 40 ~ 80 DEG C 12 ~ 48h.
The green method of a kind of functional modification nano-cellulose the most according to claim 1, it is characterised in that: step
(2) the sulfur hydrogen salt class ionic liquid in is 3:5 with the mass ratio of the ionic liquid in step (3).
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| CN108624634A (en) * | 2018-04-19 | 2018-10-09 | 华南理工大学 | A kind of method that enzyme process prepares the sugar ester analog derivative with antibacterial functions |
| CN111205397A (en) * | 2020-03-02 | 2020-05-29 | 青岛科技大学 | Ionic liquid grafted cellulose nanocrystal and preparation method thereof |
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| CN108624634A (en) * | 2018-04-19 | 2018-10-09 | 华南理工大学 | A kind of method that enzyme process prepares the sugar ester analog derivative with antibacterial functions |
| CN108624634B (en) * | 2018-04-19 | 2021-09-21 | 华南理工大学 | Method for preparing sugar ester derivative with antibacterial function by enzyme method |
| CN111205397A (en) * | 2020-03-02 | 2020-05-29 | 青岛科技大学 | Ionic liquid grafted cellulose nanocrystal and preparation method thereof |
| CN111205397B (en) * | 2020-03-02 | 2022-08-23 | 青岛科技大学 | Ionic liquid grafted cellulose nanocrystal and preparation method thereof |
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