CN109517863A - A kind of preparation method of modified hydrophilic group nano cellulose crystal - Google Patents
A kind of preparation method of modified hydrophilic group nano cellulose crystal Download PDFInfo
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- CN109517863A CN109517863A CN201811486804.1A CN201811486804A CN109517863A CN 109517863 A CN109517863 A CN 109517863A CN 201811486804 A CN201811486804 A CN 201811486804A CN 109517863 A CN109517863 A CN 109517863A
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- C12P19/00—Preparation of compounds containing saccharide radicals
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Abstract
The invention discloses a kind of preparation methods of modified hydrophilic group nano cellulose crystal, include the following steps: S1: material prepares, and chooses microcrystalline cellulose, acetic acid solution, anhydrous phosphoric acid solution, peracetic acid soln, suitable multicomponent oxide agent；S2: choosing 1 part of microcrystalline cellulose and 1 part of anhydrous phosphoric acid solution, first puts into anhydrous phosphoric acid solution in glass reaction kettle, then puts into anhydrous phosphoric acid solution microcrystalline cellulose and is stirred；S3: 1 part of acetic acid solution is put into solution obtained in step S2；S4: 2 parts of peracetic acid soln is put into toward solution obtained in step S3 and suitable multicomponent oxide agent is stirred；S4: 2 parts of peracetic acid soln is put into toward solution obtained in step S3 and suitable multicomponent oxide agent is stirred.Oxidation system of the invention is directed to cellulose different loci selective oxidation, and the oxidation efficiency of the high native cellulose of crystallinity can be improved.
Description
Technical field
The present invention relates to cellulose crystals technical field more particularly to a kind of modified hydrophilic group nano cellulose crystals
Preparation method.
Background technique
Under the increasingly depleted status of the non-renewable resources such as coal, oil and natural gas, renewable money is sufficiently developed and used
Source becomes inexorable trend.Native cellulose is the most abundant biomass resource on the earth, is that most wide biology is distributed in nature
Macromolecule, it is present in various biological such as plants, animal and some bacteriums.Nano cellulose crystal is from day
A kind of nanoscale cellulose extracted in right fiber, it not only has the feature of nano particle, also has some unique
Intensity and optical property, have broad application prospects.The preparation process of traditional nano cellulose crystal is complicated, really operates
Get up to waste raw material and manpower, greatly increases use cost.
Summary of the invention
The invention proposes a kind of preparation methods of modified hydrophilic group nano cellulose crystal, to solve above-mentioned background skill
The problem of being proposed in art.
The invention proposes a kind of preparation methods of modified hydrophilic group nano cellulose crystal, comprising the following steps:
S1: material prepares, and chooses 1~6 part of microcrystalline cellulose, wherein the quality of every part of microcrystalline cellulose is 1g, acetic acid is molten
1~15 part of liquid, the quality of acetic acid is 2.33g in every part of acetic acid solution, and cellulase is several, 1~10 part of anhydrous phosphoric acid solution, often
Part anhydrous phosphoric acid solution is 300ml, 1~10 part of peracetic acid soln, suitable multicomponent oxide agent；
S2: choosing 1 part of microcrystalline cellulose and 1 part of anhydrous phosphoric acid solution, first by the investment glass reaction of anhydrous phosphoric acid solution
In kettle, then microcrystalline cellulose is put into anhydrous phosphoric acid solution and is stirred, wherein needing to be stirred using glass stirring rod
It mixes, mixing speed is 30~40r/min, and solution is stirred to collosol state；
S3: 1 part of acetic acid solution is put into solution obtained in step S2, since the quality of acetic acid in every part of acetic acid solution is
2.33g, therefore the mass ratio of acetic acid and microcrystalline cellulose is 7:3 in the mixed solution, is then mixed, so that solution
Acetylization reaction occurs, wherein mixing speed is 20~30r/min, and wherein whipping temp is 10~20 DEG C, the reaction time 10
~15min；
S4: 2 parts of peracetic acid soln is put into toward solution obtained in step S3 and suitable multicomponent oxide agent is stirred
Processing is mixed, wherein mixing speed is 40~50r/min, and being stirred to react environment is 26~29 DEG C under the conditions of being protected from light, mixing time
For 3h, stirring puts into suitable cellulase into solution after finishing and is digested, cellulase in the solution dense
Degree is 10-15u/ml, is ultrasonically treated in enzymolysis process at interval of 12h, and each ultrasonic time is 30~60min；
S5: the sample for taking step S4 to obtain is filtered, and suction filtration is washed after finishing using deionized water, is washed repeatedly
It washs four times, wherein the water temperature of deionized water is maintained at 10~20 DEG C；
S6: carrying out centrifuge processing for product obtained in step S5, handle 2~4 times, carries out after being disposed
It is dried, drying time is 15~30min, and finished product can be obtained in drying process after finishing.
Preferred: drying process device in step S6 is desiccant, drying parameter are as follows: inlet air temperature: 10~30 DEG C,
Leaving air temp: 80~120 DEG C, wriggling pump discharge: 50~100mL/h.
Preferred: the anhydrous phosphoric acid solution is the anhydrous phosphoric acid system mixed by polyphosphoric acids and phosphoric acid solution,
Phosphorus pentoxide content is 70%~85%.
Preferred: the glass reaction kettle in step S2 is explosion-proof 100L double-layer glass reaction kettle, model PRG-100.
Preferred: the reaction in step S3 is preferably acetylation, but is not limited to acetylation, additionally it is possible to be propionating, fourth
Acylation, maleylation, laurel is acylated, grease is acylated, benzoylation either oxalyl, obtain corresponding product be it is propionating,
Butyrylation, maleylation, laurel acylation, grease acylation, benzoylation, oxalyl nano cellulose crystal, it is corresponding to use
Acylating reagent be corresponding acid anhydrides, carboxylic acid halides or acid respectively.
Preferred: the hydrogen bond base content of obtained cellulose crystals is 0.4~1.0mmol/g, and the degree of polymerization 800 is protected
Water number is 350%, and a length of 7~35 μm of crystalline size, width is 3~12nm.
A kind of preparation method of modified hydrophilic group nano cellulose crystal proposed by the present invention, beneficial effect are: this
The oxidation system of invention is directed to cellulose different loci selective oxidation, and the oxidation effect of the high native cellulose of crystallinity can be improved
Rate, nano cellulose crystal surface-bound carboxylic content, water retention value, carboxyl degree of substitution, crystallinity are significantly increased, and technique is steady
Fixed, easy to operate, the inexpensive object of raw material is rich, pollution-free, can large-scale promotion production, papermaking, food, cosmetics, electronic product,
Medical domain has good application prospect.
Specific embodiment
It is next combined with specific embodiments below that the present invention will be further described.
Embodiment 1
The invention proposes a kind of preparation methods of modified hydrophilic group nano cellulose crystal, comprising the following steps:
S1: material prepares, and chooses 1 part of microcrystalline cellulose, wherein the quality of every part of microcrystalline cellulose is 1g, acetic acid solution 1
Part, the quality of acetic acid is 2.33g in every part of acetic acid solution, and cellulase is several, 1 part of anhydrous phosphoric acid solution, every part of anhydrous phosphoric acid
Solution is 300ml, 1 part of peracetic acid soln, suitable multicomponent oxide agent；
S2: choosing 1 part of microcrystalline cellulose and 1 part of anhydrous phosphoric acid solution, first by the investment glass reaction of anhydrous phosphoric acid solution
In kettle, then microcrystalline cellulose is put into anhydrous phosphoric acid solution and is stirred, wherein needing to be stirred using glass stirring rod
It mixes, mixing speed 30r/min stirs solution to collosol state；
S3: 1 part of acetic acid solution is put into solution obtained in step S2, since the quality of acetic acid in every part of acetic acid solution is
2.33g, therefore the mass ratio of acetic acid and microcrystalline cellulose is 7:3 in the mixed solution, is then mixed, so that solution
Acetylization reaction occurs, wherein mixing speed is 20r/min, and wherein whipping temp is 10 DEG C, reaction time 10min；
S4: 2 parts of peracetic acid soln is put into toward solution obtained in step S3 and suitable multicomponent oxide agent is stirred
Processing is mixed, wherein mixing speed is 40r/min, and being stirred to react environment is 26 DEG C under the conditions of being protected from light, mixing time 3h, stirring
It puts into suitable cellulase into solution after finishing to be digested, the concentration of cellulase in the solution is 10u/
Ml is ultrasonically treated in enzymolysis process at interval of 12h, and each ultrasonic time is 30min；
S5: the sample for taking step S4 to obtain is filtered, and suction filtration is washed after finishing using deionized water, is washed repeatedly
It washs four times, wherein the water temperature of deionized water is maintained at 10 DEG C；
S6: product obtained in step S5 is subjected to centrifuge processing, is handled 2 times, is done after being disposed
Finished product can be obtained in dry processing, drying time 15min, drying process after finishing.
Drying process device in step S6 is desiccant, drying parameter are as follows: inlet air temperature: 10 DEG C, leaving air temp: 80
DEG C, wriggling pump discharge: 50mL/h.
The anhydrous phosphoric acid solution is the anhydrous phosphoric acid system mixed by polyphosphoric acids and phosphoric acid solution, five oxidations two
Phosphorus content is 70%.
Glass reaction kettle in step S2 is explosion-proof 100L double-layer glass reaction kettle, model PRG-100.
Reaction in step S3 is preferably acetylation, but is not limited to acetylation, additionally it is possible to be propionating, Butyrylation, horse
Come be acylated, laurel is acylated, grease is acylated, benzoylation either oxalyl, obtain corresponding product be propionating, Butyrylation,
Maleylation, laurel acylation, grease acylation, benzoylation, oxalyl nano cellulose crystal, the corresponding acylated examination used
Agent is corresponding acid anhydrides, carboxylic acid halides or acid respectively.
The hydrogen bond base content of obtained cellulose crystals be 0.4mmol/g, the degree of polymerization 800, water retention value 350%,
A length of 7 μm of crystalline size, width 3nm.
Embodiment 2
The invention proposes a kind of preparation methods of modified hydrophilic group nano cellulose crystal, comprising the following steps:
S1: material prepares, and chooses 6 parts of microcrystalline cellulose, wherein the quality of every part of microcrystalline cellulose is 1g, acetic acid solution 15
Part, the quality of acetic acid is 2.33g in every part of acetic acid solution, and cellulase is several, 10 parts of anhydrous phosphoric acid solution, every part of anhydrous phosphoric acid
Solution is 300ml, 10 parts of peracetic acid soln, suitable multicomponent oxide agent；
S2: choosing 1 part of microcrystalline cellulose and 1 part of anhydrous phosphoric acid solution, first by the investment glass reaction of anhydrous phosphoric acid solution
In kettle, then microcrystalline cellulose is put into anhydrous phosphoric acid solution and is stirred, wherein needing to be stirred using glass stirring rod
It mixes, mixing speed 40r/min stirs solution to collosol state；
S3: 1 part of acetic acid solution is put into solution obtained in step S2, since the quality of acetic acid in every part of acetic acid solution is
2.33g, therefore the mass ratio of acetic acid and microcrystalline cellulose is 7:3 in the mixed solution, is then mixed, so that solution
Acetylization reaction occurs, wherein mixing speed is 30r/min, and wherein whipping temp is 20 DEG C, reaction time 15min；
S4: 2 parts of peracetic acid soln is put into toward solution obtained in step S3 and suitable multicomponent oxide agent is stirred
Processing is mixed, wherein mixing speed is 50r/min, and being stirred to react environment is 29 DEG C under the conditions of being protected from light, mixing time 3h, stirring
It puts into suitable cellulase into solution after finishing to be digested, the concentration of cellulase in the solution is 15u/
Ml is ultrasonically treated in enzymolysis process at interval of 12h, and each ultrasonic time is 60min；
S5: the sample for taking step S4 to obtain is filtered, and suction filtration is washed after finishing using deionized water, is washed repeatedly
It washs four times, wherein the water temperature of deionized water is maintained at 20 DEG C；
S6: product obtained in step S5 is subjected to centrifuge processing, is handled 4 times, is done after being disposed
Finished product can be obtained in dry processing, drying time 30min, drying process after finishing.
Drying process device in step S6 is desiccant, drying parameter are as follows: inlet air temperature: 30 DEG C, leaving air temp: 20
DEG C, wriggling pump discharge: 100mL/h.
The anhydrous phosphoric acid solution is the anhydrous phosphoric acid system mixed by polyphosphoric acids and phosphoric acid solution, five oxidations two
Phosphorus content is 85%.
Glass reaction kettle in step S2 is explosion-proof 100L double-layer glass reaction kettle, model PRG-100.
Reaction in step S3 is preferably acetylation, but is not limited to acetylation, additionally it is possible to be propionating, Butyrylation, horse
Come be acylated, laurel is acylated, grease is acylated, benzoylation either oxalyl, obtain corresponding product be propionating, Butyrylation,
Maleylation, laurel acylation, grease acylation, benzoylation, oxalyl nano cellulose crystal, the corresponding acylated examination used
Agent is corresponding acid anhydrides, carboxylic acid halides or acid respectively.
The hydrogen bond base content of obtained cellulose crystals be 1.0mmol/g, the degree of polymerization 800, water retention value 350%,
A length of 35 μm of crystalline size, width 12nm.
Embodiment 3
The invention proposes a kind of preparation methods of modified hydrophilic group nano cellulose crystal, comprising the following steps:
S1: material prepares, and chooses 5 parts of microcrystalline cellulose, wherein the quality of every part of microcrystalline cellulose is 1g, acetic acid solution 10
Part, the quality of acetic acid is 2.33g in every part of acetic acid solution, and cellulase is several, 5 parts of anhydrous phosphoric acid solution, every part of anhydrous phosphoric acid
Solution is 300ml, 5 parts of peracetic acid soln, suitable multicomponent oxide agent；
S2: choosing 1 part of microcrystalline cellulose and 1 part of anhydrous phosphoric acid solution, first by the investment glass reaction of anhydrous phosphoric acid solution
In kettle, then microcrystalline cellulose is put into anhydrous phosphoric acid solution and is stirred, wherein needing to be stirred using glass stirring rod
It mixes, mixing speed 35r/min stirs solution to collosol state；
S3: 1 part of acetic acid solution is put into solution obtained in step S2, since the quality of acetic acid in every part of acetic acid solution is
2.33g, therefore the mass ratio of acetic acid and microcrystalline cellulose is 7:3 in the mixed solution, is then mixed, so that solution
Acetylization reaction occurs, wherein mixing speed is 25r/min, and wherein whipping temp is 12 DEG C, reaction time 13min；
S4: 2 parts of peracetic acid soln is put into toward solution obtained in step S3 and suitable multicomponent oxide agent is stirred
Processing is mixed, wherein mixing speed is 45r/min, and being stirred to react environment is 28 DEG C under the conditions of being protected from light, mixing time 3h, stirring
It puts into suitable cellulase into solution after finishing to be digested, the concentration of cellulase in the solution is 12u/
Ml is ultrasonically treated in enzymolysis process at interval of 12h, and each ultrasonic time is 40min；
S5: the sample for taking step S4 to obtain is filtered, and suction filtration is washed after finishing using deionized water, is washed repeatedly
It washs four times, wherein the water temperature of deionized water is maintained at 15 DEG C；
S6: product obtained in step S5 is subjected to centrifuge processing, is handled 3 times, is done after being disposed
Finished product can be obtained in dry processing, drying time 20min, drying process after finishing.
Drying process device in step S6 is desiccant, drying parameter are as follows: inlet air temperature: 15 DEG C, leaving air temp: 85
DEG C, wriggling pump discharge: 60mL/h.
The anhydrous phosphoric acid solution is the anhydrous phosphoric acid system mixed by polyphosphoric acids and phosphoric acid solution, five oxidations two
Phosphorus content is 75%.
Glass reaction kettle in step S2 is explosion-proof 100L double-layer glass reaction kettle, model PRG-100.
Reaction in step S3 is preferably acetylation, but is not limited to acetylation, additionally it is possible to be propionating, Butyrylation, horse
Come be acylated, laurel is acylated, grease is acylated, benzoylation either oxalyl, obtain corresponding product be propionating, Butyrylation,
Maleylation, laurel acylation, grease acylation, benzoylation, oxalyl nano cellulose crystal, the corresponding acylated examination used
Agent is corresponding acid anhydrides, carboxylic acid halides or acid respectively.
The hydrogen bond base content of obtained cellulose crystals be 0.5mmol/g, the degree of polymerization 800, water retention value 350%,
A length of 2035 μm of crystalline size, width 4nm.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of modified hydrophilic group nano cellulose crystal, which comprises the following steps:
S1: material prepare, choose 1~6 part of microcrystalline cellulose, wherein the quality of every part of microcrystalline cellulose be 1g, acetic acid solution 1~
15 parts, the quality of acetic acid is 2.33g in every part of acetic acid solution, and cellulase is several, 1~10 part of anhydrous phosphoric acid solution, every part of nothing
Water phosphoric acid solution be 300ml, 1~10 part of peracetic acid soln, suitable multicomponent oxide agent；
S2: choosing 1 part of microcrystalline cellulose and 1 part of anhydrous phosphoric acid solution, first puts into anhydrous phosphoric acid solution in glass reaction kettle,
Then microcrystalline cellulose is put into anhydrous phosphoric acid solution and is stirred, wherein needing to be stirred using glass stirring rod, is stirred
Mixing speed is 30~40r/min, and solution is stirred to collosol state；
S3: 1 part of acetic acid solution is put into solution obtained in step S2, since the quality of acetic acid in every part of acetic acid solution is
2.33g, therefore the mass ratio of acetic acid and microcrystalline cellulose is 7:3 in the mixed solution, is then mixed, so that solution
Acetylization reaction occurs, wherein mixing speed is 20~30r/min, and wherein whipping temp is 10~20 DEG C, the reaction time 10
~15min；
S4: 2 parts of peracetic acid soln is put into toward solution obtained in step S3 and suitable multicomponent oxide agent is stirred place
Reason, wherein mixing speed is 40~50r/min, and being stirred to react environment is 26~29 DEG C under the conditions of being protected from light, mixing time 3h,
Stirring puts into suitable cellulase into solution after finishing and is digested, and the concentration of cellulase in the solution is
10-15u/ml is ultrasonically treated in enzymolysis process at interval of 12h, and each ultrasonic time is 30~60min；
S5: the sample for taking step S4 to obtain is filtered, and suction filtration is washed after finishing using deionized water, washs four repeatedly
Secondary, wherein the water temperature of deionized water is maintained at 10~20 DEG C；
S6: product obtained in step S5 is subjected to centrifuge processing, is handled 2~4 times, is dried after being disposed
Processing, drying time are 15~30min, and finished product can be obtained in drying process after finishing.
2. a kind of preparation method of modified hydrophilic group nano cellulose crystal according to claim 1, it is characterised in that:
Drying process device in step S6 is desiccant, drying parameter are as follows: inlet air temperature: 10~30 DEG C, leaving air temp: 80~
120 DEG C, wriggling pump discharge: 50~100mL/h.
3. a kind of preparation method of modified hydrophilic group nano cellulose crystal according to claim 1, it is characterised in that:
The anhydrous phosphoric acid solution is the anhydrous phosphoric acid system mixed by polyphosphoric acids and phosphoric acid solution, and phosphorus pentoxide content is
70%~85%.
4. a kind of preparation method of modified hydrophilic group nano cellulose crystal according to claim 1, it is characterised in that:
Glass reaction kettle in step S2 is explosion-proof 100L double-layer glass reaction kettle, model PRG-100.
5. a kind of preparation method of modified hydrophilic group nano cellulose crystal according to claim 1, it is characterised in that:
Reaction in step S3 is preferably acetylation, but is not limited to acetylation, additionally it is possible to be propionating, Butyrylation, maleylation, the moon
Osmanthus is acylated, grease is acylated, benzoylation either oxalyl, obtain corresponding product be propionating, Butyrylation, maleylation,
Laurel acylation, grease acylation, benzoylation, oxalyl nano cellulose crystal, the corresponding acylating reagent used is respectively
Corresponding acid anhydrides, carboxylic acid halides or acid.
6. a kind of preparation method of modified hydrophilic group nano cellulose crystal according to claim 1, it is characterised in that:
The hydrogen bond base content of obtained cellulose crystals is 0.4~1.0mmol/g, the degree of polymerization 800, water retention value 350%, crystal
A length of 7~35 μm of size, width is 3~12nm.
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Cited By (1)
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| CN115819848A (en) * | 2022-11-28 | 2023-03-21 | 浙江大学 | Multifunctional nano-cellulose composite solution and preparation method and application thereof |
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Cited By (2)
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| CN115819848A (en) * | 2022-11-28 | 2023-03-21 | 浙江大学 | Multifunctional nano-cellulose composite solution and preparation method and application thereof |
| CN115819848B (en) * | 2022-11-28 | 2024-04-30 | 浙江大学 | Multifunctional nano-cellulose composite solution and preparation method and application thereof |
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Application publication date: 20190326 |