CN109206666A - A kind of nanocrystal cellulose aquagel and preparation method thereof - Google Patents
A kind of nanocrystal cellulose aquagel and preparation method thereof Download PDFInfo
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- CN109206666A CN109206666A CN201810388752.8A CN201810388752A CN109206666A CN 109206666 A CN109206666 A CN 109206666A CN 201810388752 A CN201810388752 A CN 201810388752A CN 109206666 A CN109206666 A CN 109206666A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21B1/00—Fibrous raw materials or their mechanical treatment
- D21B1/02—Pretreatment of the raw materials by chemical or physical means
- D21B1/021—Pretreatment of the raw materials by chemical or physical means by chemical means
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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Abstract
The invention discloses a kind of nanocrystal cellulose aquagels and preparation method thereof, select common on the market agriculture and forestry organic waste material Eucalyptus and filter paper, Eucalyptus Fibers element is mentioned using three kinds of nitric acid-sodium-hydroxide method, nitric acid-Ethanol Method and tetrahydrofuran-water-soluble fluorine methods, filter paper fibre element is extracted using sodium hydroxide alkalization and acid-hydrolysis method and tetrahydrofuran-water-soluble fluorine.It is preferred that recovery rate is higher when tetrahydrofuran-water-soluble fluorine extracts.The cellulose of said extracted is prepared into nanocrystal cellulose aquagel, good compared to general hydrogel gel stability, moderate viscosity is not easily settled, has more superior property.
Description
Technical field
The present invention relates to the technical fields more particularly to a kind of utilization agriculture and forestry organic waste material of life science and new material to prepare
Nanocrystal cellulose aquagel, which has the characteristics that environmentally friendly, nontoxic, harmless, Ke Yizuo
For the basic material of the equipment more demanding to human compatibility such as wearable smart machine.
Background technique
1769, after James's watt improvement steam engine has caused the industrial revolution, industrial production, the science of human society
Technology and quality of life achieve huge promotion.It is 50 years especially nearly, global economy and rapid industrial development, at this
A presumption principle vital factor in behind is exactly high-tech bring a series of new material.However, these new materials
Often by artificial synthesized, such as macromolecule polypropylene, polystyrene and substance containing chromium, these substances are often difficult to degrade and contain
It is toxic, cause serious environmental pollution.For this purpose, can protect the investigation of materials of human health and environment, exploitation and application
Have become a focus.
Cellulose is mainly formed by photosynthesis of plant, has many advantages, such as nontoxic, degradable.Recently as
Petroleum, the decline of coal reserves and oil price are skyrocketed through, with various countries' environmental pollution growing interest and
Pay attention to, the application of the regenerated resources of this sustainable development of cellulose is increasingly taken seriously.
China is the current maximum country of agricultural wastes quantum of output in the world.Largely discarded agricultural product not only cause
The serious waste of resource, and also pollute the environment if dealt with improperly, in some instances it may even be possible to cause food-safety problem.Therefore, originally
Invention has chosen two kinds of agriculture and forestry organic waste material filter paper and Eucalyptus, the cellulose recovery rate and partial size gone out by comparing extraction by different technology
Etc. parameters, effective recycling and reusing is carried out to agriculture and forestry organic waste material, finally extracts nanocrystal cellulose, and using extracting
Cellulose out prepares hydrogel, can not only reduce great economic loss caused by agriculture and forestry organic waste material, improves resource reutilization
Level, and the livelihood issues such as food-safe and environmental improvement, will all play direct or indirect contribution.
Summary of the invention
The purpose of the present invention is the recycling and reusings by agriculture and forestry organic waste material, provide a kind of nanocrystal cellulose aquagel
And preparation method thereof, which has the characteristics that environmentally friendly, nontoxic, harmless, stability is good, can be used as
The basic material of the equipment more demanding to human compatibility such as wearable smart machine.
A kind of nanocrystal cellulose aquagel and preparation method thereof, the present invention have chosen relatively common on the market two kinds
Agriculture and forestry organic waste material is Eucalyptus and filter paper respectively.Eucalyptus is the discarded corncob in Beijing area, and filter paper is laboratory abandoned filter paper.
It is water-soluble that nitric acid-sodium-hydroxide method, nitric acid-Ethanol Method and tetrahydrofuran-is respectively adopted in Eucalyptus Fibers element extracting method
Three kinds of methods of agent method are extracted.It is preferred that recovery rate is higher when tetrahydrofuran-water-soluble fluorine extracts.
Sodium hydroxide alkalization is respectively adopted in filter paper fibre element extracting method and acid-hydrolysis method and tetrahydrofuran-water-soluble fluorine mention
It takes.It is preferred that the extraction pollution of tetrahydrofuran method is lower, more environmentally-friendly.
Gel is prepared by the nanocrystal cellulose of said extracted, viscosity good compared to general hydrogel gel stability
It is moderate, it is not easily settled, there is more superior property.The gel extracted is transparent gluey hydrogel, need to be placed on from
It is saved in sub- water.
Detailed description of the invention
Fig. 1 gel electro kinetic potential measurement result figure
Specific embodiment
Eucalyptus Fibers element extracting method；Using nitric acid-sodium-hydroxide method, nitric acid-Ethanol Method or tetrahydrofuran-water-soluble fluorine
It extracts.
Nitric acid-sodium-hydroxide method；
35g Eucalyptus powder is taken, the sodium hydroxide solution that PH is 12 is added, holding solid-to-liquid ratio is 1: 20 (g/mL), at 60 DEG C
Constant temperature 75min under water-bath distills water washing, filters, and dries in baking oven.The powder of above-mentioned drying is taken, it is molten that the nitric acid that pH is 3 is added
Liquid, solid-to-liquid ratio 1: 20 (g/mL), the constant temperature 75min under 60 DEG C of water-baths, distilled water washing are filtered, are dried in baking oven, and eucalyptus is both obtained
Lignose.
Nitric acid-Ethanol Method:
It takes 35g to irradiate Eucalyptus powder, is put into clean conical flask, nitric acid-alcohol mixeding liquid is added, loads onto condensing reflux
Pipe, boiling water bath are heated to powder and bleach.Residue is washed with nitric acid-alcohol mixeding liquid, reusable heat water washing to neutrality finally uses nothing
Water-ethanol washs 2 times, filters, and drying is to get Eucalyptus Fibers element.
The cellulose that said extracted goes out is placed in 100ml three-necked flask, is fixed on the iron stand equipped with blender, puts
Enter in thermostat water bath, be slowly dropped into the sulfuric acid solution (sulfuric acid solution is 30: 1 with cellulose mass ratio) prepared and stirred
It mixes.After reaction 8 hours, deionized water (deionized water is about 5: 1 with reaction mixture volume ratio) is added and stops reacting.With ultrasound
Shaker ultrasonication stands a few hours after 90 minutes, supernatant is discharged, and carries out centrifuge washing, every centrifugation 1 to lower sediment
It is secondary, the supernatant in centrifuge tube is discharged, centrifuge washing again after being mixed to lower sediment plus water, centrifuge speed 300r/min,
The suspension washed repeatedly into centrifuge tube no longer settles.Suspension is moved into bag filter and is put into deionized water
In, the retention relative molecular mass of bag filter is 8000-14000, so can stay in bag.Obtain Eucalyptus nanocrystal fiber
Element.
Tetrahydrofuran-water-soluble fluorine:
With the mixed solution (volume ratio 6: 4) of 350ml tetrahydrofuran and water.Eucalyptus powder 35g. is added and is placed in high temperature height
It presses in reaction kettle, temperature is 170 DEG C, revolving speed 400r/min, pressure 100Mpa, the reaction time 1 hour.Mixed solution is filtered,
The mixed solution (volume ratio 3: 2) of filter residue tetrahydrofuran and water is washed 3 times, is then washed with deionized 3 times.It is placed in
It in conical flask, is bleached with 6.25ml sodium hypochlorite and 0.5g sodium hydroxide and deionized water, solid-to-liquid ratio 1: 20. is placed in shaking table
Reaction, condition are 50 DEG C, and the time is 2 hours.It repeats blanching step 3 times, puts into a centrifuge centrifugation until supernatant pH value
For neutrality.The solution for being finally 0.5% by obtained solution allocation, 1 hour of ultrasonic vibration.It is outstanding up to nanocrystal cellulose
Turbid.
Filter paper fibre element extracting method: it is extracted using sodium hydroxide alkalization and acid-hydrolysis method or tetrahydrofuran-water-soluble fluorine.
Sodium hydroxide alkalization and acid-hydrolysis method:
At room temperature, basification 1h is carried out to filter paper with 30% sodium hydroxide solution, then is washed repeatedly with deionized water
It washs, filters.Alkalization sawdust is dried to permanent quality in 90 DEG C of drying boxes to get cellulose.
It is washed with distilled water to neutrality the cellulose extracted is placed in 100ml three-necked flask, be fixed on equipped with stirring
It on the iron stand of device, is put into thermostat water bath, being slowly dropped into the sulfuric acid solution for preparing, (sulfuric acid solution is with cellulose mass ratio
30: 1) and being stirred.After reaction 8 hours, deionized water (deionized water and reaction mixture volume ratio are about 5: 1) is added and stops
Only react.With a few hours are stood after sonic oscillation instrument ultrasonication 100 minutes, supernatant is discharged, to lower sediment carry out from
Heart washing, every centrifugation 1 time, is discharged the supernatant in centrifuge tube, centrifuge washing again after mixing to lower sediment plus water, centrifugal basket
Speed is 300r/min, and the suspension washed repeatedly into centrifuge tube no longer settles.Suspension is moved into bag filter simultaneously
It is put into deionized water, the retention relative molecular mass of bag filter is 8000~14000, so can stay in bag.Obtain nanometer
Avicel cellulose.
Tetrahydrofuran-water-soluble fluorine:
With the mixed solution (volume ratio 6: 4) of 350ml tetrahydrofuran and water.Filter paper is added, is placed in high-temperature high-voltage reaction
In kettle, temperature is 170 DEG C, revolving speed 400r/min, pressure 100Mpa, the reaction time 1 hour.Mixed solution is filtered, by filter residue
It is washed 3 times, is then washed with deionized 3 times with the mixed solution (volume ratio 3: 2) of tetrahydrofuran and water.It is placed in conical flask
In, it is bleached with 6.25ml sodium hypochlorite and 0.5g sodium hydroxide and deionized water, solid-to-liquid ratio 1: 20., which is placed in shaking table, reacts,
Condition is 50 DEG C, and the time is 2 hours.It repeats blanching step 2 times, puts into a centrifuge centrifugation until during supernatant pH value is
Property.The solution for being finally 0.5% by obtained solution allocation, 1 hour of ultrasonic vibration.It is suspended up to nanocrystal cellulose
Liquid.
Gel is manufactured using the nanocrystal cellulose extracted:
This experiment takes Eucalyptus nanocrystal cellulose mentioned above to prepare gel, with 20ml dimethyl sulfoxide (DMSO)
It is that solution and 1.2g (PVA) are configured to solution with 3: 2 proportional arrangement of water.Under 90 DEG C of water bath conditions, mechanical stirring speed
300r/min, time are 2 hours.Mixed solution is taken out, 10mg CNC is poured into, is continued under 90 DEG C of water bath conditions, machinery stirs
Mixing speed to be is 1 hour the 300r/min. time.Mixed solution is poured on plate, nature gel is allowed to.Plate is placed in ice
In case, temperature is -3 DEG C, and the time is 24 hours.Take out gel, by merging bag filter in, bag outside be deionized water.With going
The continuous replacement of ionized water, organic solvent can gradually decrease.After 2 days, gel is taken out, is placed in deionized water, freezen protective.
It is that the discarded cellulose recovery rate extracted of different agricultural compares below:
By carrying out accurate measurement to experiment front and back sample quality, the data about recovery rate obtained are as shown in the table:
By the analysis to data in table, it is seen that: when extracting Eucalyptus Fibers element, mentioned with tetrahydrofuran-water-soluble fluorine
Rate highest, followed by nitric acid-Ethanol Method are taken, nitric acid-sodium-hydroxide method recovery rate is minimum.And extracting the cellulose in filter paper
When, acid-hydrolysis method can a little higher than solvent method.If consider error, when extracting filter paper fibre element, tetrahydrofuran-water-soluble fluorine and
Traditional acid-hydrolysis method recovery rate is not much different, but solvent method pollution is lower, and the industry that is more suitable is used with laboratory.
Below by way of the gel feature for carrying out electro kinetic potential measurement observation preparation to gel:
Gel electro kinetic potential measurement result such as Fig. 1:
Pass through observation analysis, it can be deduced that, the electro kinetic potential of gel is higher (being higher than 50mV), thus illustrates nanocrystal fibre
Dimension element is solution-stabilized to be settled, and thus obtained gel is relatively uniform, and stability is very good.
By the analysis of electro kinetic potential for gel, it can be found that: the nanocrystal cellulose granules in gel have compared with
High electro kinetic potential (up to 71mv), the hydrogel that higher electro kinetic potential will lead to the formation of nanocrystal cellulose have
Good stability.It is 2.52mpa.s by the gel viscosity that the viscosimetric analysis discovery to gel extracts.It is such glutinous
It spends moderate, causes gel very frangible while will not be excessively sticky.The superior material compatible with human body can be become.
Claims (10)
1. a kind of nanocrystal cellulose aquagel and preparation method thereof, it is characterised in that: select agriculture and forestry organic waste material Eucalyptus and filter
Paper extracts cellulose and prepares nanocrystal cellulose aquagel.
2. a kind of nanocrystal cellulose aquagel and preparation method thereof as described in claim 1, it is characterised in that: the Eucalyptus
Cellulose extracting method is to be extracted using nitric acid-sodium-hydroxide method, nitric acid-Ethanol Method or tetrahydrofuran-water-soluble fluorine.
3. a kind of nanocrystal cellulose aquagel and preparation method thereof as described in claim 1, it is characterised in that: the filter paper
Cellulose extracting method is to be extracted using sodium hydroxide alkalization and acid-hydrolysis method or tetrahydrofuran-water-soluble fluorine.
4. a kind of nanocrystal cellulose aquagel and preparation method thereof as claimed in claim 2, it is characterised in that: the nitre
Acid-sodium-hydroxide method is specifically, take 35g Eucalyptus powder, and the sodium hydroxide solution that addition PH is 12, keeping solid-to-liquid ratio is 1: 20
(g/mL), the constant temperature 75min under 60 DEG C of water-baths distills water washing, filters, and dries in baking oven；The powder of above-mentioned drying is taken, is added
The nitric acid solution that pH is 3, solid-to-liquid ratio 1: 20 (g/mL), the constant temperature 75min under 60 DEG C of water-baths, distilled water washing filtering, baking oven
Middle drying had both obtained Eucalyptus Fibers element.
5. a kind of nanocrystal cellulose aquagel and preparation method thereof as claimed in claim 2, it is characterised in that: the nitre
Acid-Ethanol Method specifically, take 35g irradiate Eucalyptus powder, be put into clean conical flask, be added nitric acid-alcohol mixeding liquid, load onto
Condensing reflux pipe, boiling water bath are heated to powder and bleach；Residue is washed with nitric acid-alcohol mixeding liquid, reusable heat water washing to neutrality,
It is finally washed 2 times, is filtered with dehydrated alcohol, drying is to get Eucalyptus Fibers element.
The cellulose that said extracted goes out is placed in 100ml three-necked flask, is fixed on the iron stand equipped with blender, is put into perseverance
In warm water bath, it is slowly dropped into the sulfuric acid solution prepared, sulfuric acid solution and cellulose mass ratio are 30: 1, and are stirred；Instead
After answering 8 hours, deionized water (deionized water is about 5: 1 with reaction mixture volume ratio) is added and stops reacting；Use sonic oscillation
Instrument ultrasonication stands a few hours after 90 minutes, supernatant is discharged, and carries out centrifuge washing, every centrifugation 1 time, row to lower sediment
Supernatant in centrifuge tube out, centrifuge washing, centrifuge speed 300r/min are so anti-again after mixing to lower sediment plus water
After backwashing is washed the suspension into centrifuge tube and is no longer settled；Suspension is moved into bag filter and is put into deionized water, is dialysed
The retention relative molecular mass of bag is 8000-14000, so can stay in bag；Obtain Eucalyptus nanocrystal cellulose.
6. a kind of nanocrystal cellulose aquagel and preparation method thereof as claimed in claim 2, it is characterised in that: the tetrahydro
Furans-water-soluble fluorine is specifically, with the mixed solution of 350ml tetrahydrofuran and water, volume ratio 6: 4；Eucalyptus powder is added
35g. is placed in high-temperature high-pressure reaction kettle, temperature be 170 DEG C, revolving speed 400r/min, pressure 100Mpa, the reaction time 1 hour,
Mixed solution is filtered, by the mixed solution of filter residue tetrahydrofuran and water, volume ratio 3: 2 washs 3 times, then uses deionization
Water washing 3 times；It is placed in conical flask, is bleached with 6.25ml sodium hypochlorite and 0.5g sodium hydroxide and deionized water, solid-to-liquid ratio 1
: 20. are placed in shaking table and react, and condition is 50 DEG C, and the time is 2 hours；It repeats blanching step 3 times, puts into a centrifuge centrifugation
Until supernatant pH value is neutrality；The solution for being finally 0.5% by obtained solution allocation, 1 hour of ultrasonic vibration；It receives to obtain the final product
Rice avicel cellulose suspension.
7. a kind of nanocrystal cellulose aquagel and preparation method thereof as claimed in claim 3, it is characterised in that: the hydrogen-oxygen
Change sodaization and acid-hydrolysis method specifically, at room temperature, carrying out basification 1h to filter paper with 30% sodium hydroxide solution, then
It is washed, is filtered repeatedly with deionized water；Alkalization sawdust is dried to permanent quality in 90 DEG C of drying boxes to get cellulose.
It is washed with distilled water to neutrality the cellulose extracted is placed in 100ml three-necked flask, be fixed on equipped with blender
It on iron stand, is put into thermostat water bath, is slowly dropped into the sulfuric acid solution prepared, sulfuric acid solution and cellulose mass ratio are 30:
1, and be stirred；After reaction 8 hours, deionized water is added, deionized water and reaction mixture volume ratio are about 5: 1, are stopped
Reaction；With a few hours are stood after sonic oscillation instrument ultrasonication 100 minutes, supernatant is discharged, lower sediment is centrifuged
Washing, every centrifugation 1 time, is discharged the supernatant in centrifuge tube, centrifuge washing again after mixing to lower sediment plus water, centrifuge speed
For 300r/min, the suspension washed repeatedly into centrifuge tube is no longer settled；Suspension is moved into bag filter and is put
Enter in deionized water, the retention relative molecular mass of bag filter is 8000~14000, so can stay in bag, obtains nano junction
Crystalline cellulose.
8. a kind of nanocrystal cellulose aquagel and preparation method thereof as claimed in claim 3, it is characterised in that: the tetrahydro
Furans-water-soluble fluorine is specifically, with the mixed solution of 350ml tetrahydrofuran and water, volume ratio 6: 4；Filter paper is added, is placed in height
In warm autoclave, temperature is 170 DEG C, revolving speed 400r/min, pressure 100Mpa, the reaction time 1 hour；It is molten to filter mixing
Liquid, by the mixed solution of filter residue tetrahydrofuran and water, volume ratio 3: 2 is washed 3 times, is then washed with deionized 3 times；
It is placed in conical flask, is bleached with 6.25ml sodium hypochlorite and 0.5g sodium hydroxide and deionized water, solid-to-liquid ratio 1: 20., which is placed in, shakes
It is reacted in bed, condition is 50 DEG C, and the time is 2 hours；It repeats blanching step 2 times, puts into a centrifuge centrifugation until supernatant
PH value is neutrality；The solution for being finally 0.5% by obtained solution allocation, 1 hour of ultrasonic vibration；Up to nanocrystal fiber
Plain suspension.
9. a kind of nanocrystal cellulose aquagel and preparation method thereof as described in claim 1-8 any one, feature exists
In: it takes the Eucalyptus nanocrystal cellulose to prepare gel, is matched with 20ml dimethyl sulfoxide (DMSO) and water with 3: 2 ratio
It is set to solution and 1.2g (PVA) is configured to solution；Under 90 DEG C of water bath conditions, mechanical stirring speed 300r/min, the time 2
A hour；Mixed solution is taken out, 10mg CNC is poured into, is continued under 90 DEG C of water bath conditions, mechanical stirring speed is 300r/min.
Time is 1 hour；Mixed solution is poured on plate, nature gel is allowed to；Plate is placed in refrigerator, temperature is -3 DEG C,
Time is 24 hours；Take out gel, by merging bag filter in, bag outside be deionized water；With the continuous replacement of deionized water,
Organic solvent can gradually decrease；After 2 days, gel is taken out, is placed in deionized water, freezen protective.
10. a kind of nanocrystal cellulose aquagel, it is characterised in that: using a kind of as described in claim 1-9 any one
The preparation method of nanocrystal cellulose aquagel is prepared.
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| CN112094441A (en) * | 2019-06-18 | 2020-12-18 | 中国科学技术大学 | Composite board based on nanocellulose and preparation method thereof |
| CN112175144A (en) * | 2020-09-30 | 2021-01-05 | 上海交通大学 | Preparation method of multiple-response hydrogel based on compounding of natural polymer and synthetic polymer |
| CN113026405A (en) * | 2021-03-03 | 2021-06-25 | 西南交通大学 | Method for synchronously preparing nano lignin particles and nano cellulose fibers from agriculture and forestry biomass raw materials |
| CN116790021A (en) * | 2023-04-26 | 2023-09-22 | 辽宁丽天新材料有限公司 | Preparation process of environment-friendly expandable composite graphite flame-retardant polystyrene beads |
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| CN112094441A (en) * | 2019-06-18 | 2020-12-18 | 中国科学技术大学 | Composite board based on nanocellulose and preparation method thereof |
| CN112175144A (en) * | 2020-09-30 | 2021-01-05 | 上海交通大学 | Preparation method of multiple-response hydrogel based on compounding of natural polymer and synthetic polymer |
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| CN116790021A (en) * | 2023-04-26 | 2023-09-22 | 辽宁丽天新材料有限公司 | Preparation process of environment-friendly expandable composite graphite flame-retardant polystyrene beads |
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