CN109053906A - A kind of preparation method of nano-cellulose fiber dry powder - Google Patents
A kind of preparation method of nano-cellulose fiber dry powder Download PDFInfo
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- CN109053906A CN109053906A CN201811050809.XA CN201811050809A CN109053906A CN 109053906 A CN109053906 A CN 109053906A CN 201811050809 A CN201811050809 A CN 201811050809A CN 109053906 A CN109053906 A CN 109053906A
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- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
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- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
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Abstract
The present invention relates to a kind of preparation methods of nano-cellulose fiber dry powder, have follow steps: 1) taking cellulose, are crushed, are dried to obtain cellulosic material, for use；2) it takes organic acid and alcohol to mix, obtains reaction solution, the mass fraction of organic acid is 20-30% in reaction solution, and reaction solution is heated to 140-160 DEG C, and the cellulosic material that step 1) obtains, heat preservation, stirring is added；3) after cellulosic material is sufficiently destroyed and is dispersed, reaction system carries out solid-liquid separation treatment, obtains reaction recovered liquid and solid powder, solid powder are dispersed in alcohol after alcohol washs, obtain solid powder dispersion liquid；4) the solid powder dispersion liquid for obtaining step 3) obtains nano-cellulose fiber dispersion liquid through homogenize process；5) alcohol being evaporated in step 4) nano-cellulose fiber dispersion liquid, obtains nano-cellulose fiber dry powder.
Description
Technical field
The present invention relates to cellulose process field, in particular to a kind of preparation method of nano-cellulose fiber dry powder.
Background technique
Cellulose be by glucose group at macromolecular polysaccharide, be that one kind most wide, that content is most are distributed in nature is more
Sugar is widely present in the metabolite of plant and part bacterium, is valuable natural reproducible resource.
Crystal region and the unordered stacking stacked in the microstructure of cellulose fibre there is macromolecular ordered arrangement it is non-
Crystal region, wherein crystal region physics, chemical property are more stable.Thus, smaller szie is obtained by the destruction to noncrystalline domain
Cellulosic material, i.e. nano cellulose material.
Cellulosic material at the nanoscale has the specific physical and change for being different from cellulosic material under larger size
Performance is learned, food, biomedicine, automobile manufacture, aerospace, 3D printing, building, the special material of military project can be further applied
The fields such as material, electronic product, cosmetics, coating, paint, papermaking, composite material and enhancing by polymer.Before huge application
Scape and economic value, it is more and more to be reported out for the application of cellulose nano material and volume production exploration.
In existing reported cellulose nano material manufacturing method, chemical method, physical method, biology are specifically included that
Method etc. is a variety of.Specifically there are biologic enzymolysis method, ultrasonic method, homogeneous method, polishing, ball-milling method, acid hydrolyzation, TEMPO oxidizing process etc..
The common ground of these methods is that water consumption is big in preparation process, and products made thereby is the aqueous dispersions of cellulose nano material, product
Major defect are as follows: vulnerable to microbial contamination, height is required to storage temperature, product is long placed in and easily undergoes phase transition and settle, transportation cost
Height, application conditions are restricted in water, and product has the property of colloid, thus has and similarly easily destroyed by electrolyte with colloid
The defect of stability.
Existing nano cellulose material dry powder technology of preparing or operation sequence complexity or dispersing agent use ionic liquid etc.
Cause expensive and more harsh to reaction condition requirement, is unfavorable for the cost control in amplification quantity postpartum, uses solvent toxicity
It is higher larger to environmental hazard.Therefore, how simply, inexpensive, environmentally friendly preparation nano cellulose material, be art technology
Personnel's urgent problem to be solved.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of at low cost, reaction controllabilitys by force, cellulose is received
The anhydrous preparation method that rice material yield is high, product is dry powder-shaped.
The technical scheme is that the preparation method of nano-cellulose fiber dry powder, which is characterized in that have following step
It is rapid:
1) cellulose is taken, crushed, be dried to obtain cellulosic material, for use；
2) it takes organic acid and alcohol to mix, obtains reaction solution, the mass fraction of organic acid is 20-30%, reaction in reaction solution
Liquid is heated to 140-160 DEG C, and the cellulosic material that step 1) obtains, heat preservation, stirring is added；
3) after cellulosic material is sufficiently destroyed and is dispersed, reaction system carries out solid-liquid separation treatment, obtains reaction recycling
Liquid and solid powder, solid powder are dispersed in alcohol after alcohol washs, and obtain solid powder dispersion liquid；
4) the solid powder dispersion liquid for obtaining step 3) obtains nano-cellulose fiber dispersion liquid through homogenize process；
5) alcohol being evaporated in step 4) nano-cellulose fiber dispersion liquid, obtains nano-cellulose fiber dry powder.
Cellulose described in step 1), selected from rich cellulose-containing plant slurry, it is preferred that select wood pulp or bamboo pulp, powder
It is broken to 200 mesh；Alternatively, cellulosic material described in step 1) is purified cotton, the viscosity of purified cotton is not higher than 40mPas.
Organic acid described in step 2) is thermal decomposition temperature not less than 160 DEG C and the unitary of alcohol favorable solubility or polynary nothing
Water small molecule acid, the organic acid are citric acid, ethanedioic acid, malonic acid, succinic acid, maleic acid, benzene sulfonic acid, monoxone,
Or sour one or more mixture described above.
Alcohol described in step 2) is that boiling point is higher than 160 DEG C of unitary or polynary small molecular alcohol, and the alcohol is ethylene glycol, the third two
Alcohol, butanediol, n-octyl alcohol, pentanediol, or the mixture that alcohol described above is one or more.
The quality and reaction solution volume ratio that cellulosic material is added in step 2) are 1g:80-150mL.
In step 2) heating, insulating process, keep being condensed back.
Washing is recycled with alcohol in step 3), and washing alcohol, dispersion alcohol are not form colloidal with cellulosic material
Dispersion liquid, can dispersive cellulose material and boiling point be lower than 100 DEG C of small molecule alcohol, it is preferred that washing alcohol, dispersion alcohol
It for ethyl alcohol, is dispersed in alcohol, the solid powder quality and alcohol volume ratio of dispersion are 1g:450-1000mL.
Reaction system described in step 3) carries out solid-liquid separation treatment after being cooled to room temperature.
Homogenize process described in step 4) is to handle solid powder dispersion liquid through high pressure homogenizer, high pressure homogenizer
Processing pressure be 20000-45000psi, homogenization speed be 30mL/min.
The present invention also provides a kind of nano-cellulose dry powder, are made using any preparation method as above, the nanometer
Diameter≤100nm of cellulose dry powder, length >=200nm, the redisperse rate in pure water are 15-25%.
It has the advantages that by adopting the above technical scheme
1, the method that the present invention prepares nano-cellulose fiber dry powder, whole preparation process is anhydrous, operates without centrifugal treating,
Conducive to industrialization large-scale production, each step parameter control of preparation method is simple, mild, nano-cellulose fiber dry powder
Rate be not less than 80% (being specifically dependent upon type of feed), gained dry powder in water simple redisperse redisperse rate be 15-25%.
The nano-cellulose fiber dry powder size being prepared is distributed stable, reproducible, the more traditional side of nano-cellulose fiber dry powder
The aqueous dispersions of method preparation are easier to save and transport, and have widened the practical ranges of nano-cellulose fiber, have no longer limited to
In aqueous phase system, the product type that can be prepared is enriched.In biological medicine, papermaking, 3D printing, food and life science
It can be used as chelating agent, couplant, the agent of guarantor's type, reinforcing agent, solubilizer, thickener and excipient etc., have huge application latent
Power.
2, the nano-cellulose fiber aqueous dispersions of conventional method preparation, no matter using be evaporated, be lyophilized, supercritical drying,
The methods of atomization drying not can avoid the coalescence or film forming of nano-cellulose fiber, lose the characteristic and function of nano material.
The drying process of nano-cellulose fiber dispersion liquid is simply rapid in the present invention, and only need to be evaporated alcohol dispersion liquid can be obtained Nanowire
The dry powder of cellulose fiber effectively avoids the coalescence and film forming of nano-cellulose fiber.
3, cellulosic material of the invention first passes through 140-160 DEG C of reaction solution processing, and reaction solution is mixed by alcohol, organic acid
It is made, cellulosic material carries out alcoholysis reaction in reaction solution, damages to cellulosic material, reduces cellulosic material ruler
Very little, the mass fraction by organic acid in control reaction solution is 20-30%, prevents cellulose excessive degradation from generating levulic acid
Ester, the alcohol in reaction solution are also used for a small amount of lignin impurity contained in dissolution cellulosic material, a small amount of by-product of generation
Also it is dissolved in the alcohol of reaction solution, so that low through being separated by solid-liquid separation obtained solid powder impurity content.If reacting liquid temperature is lower than
140 DEG C, then alcoholysis reaction can not be normally carried out, and cellulosic material extent of the destruction is inadequate, oversized, in high-pressure homogeneous processing
Occluding device pipeline；If reacting liquid temperature is higher than 160 DEG C, it will lead to alcohol used or acid occur thermal decomposition and makes reaction can not be suitable
Benefit carries out or alcoholysis reaction excessively acutely reduces final product yield.Using homogenizing after the washed dispersion of solid powder
When processing, high pressure homogenizer can be passed through, obtains that purity is very high, size is distributed stable nano-cellulose fiber.
4, preparation method of the present invention, reaction solution (alcohol+organic acid), cleaning solution (alcohol), the alcohol being evaporated are using conventional hand
Section recycles, since the thermal capacitance of reaction solution (alcohol+organic acid) system is significantly reduced compared with water, energy consumption declines when heating, can
The cost of production nano-cellulose fiber dry powder is greatly reduced.
It is further described with reference to the accompanying drawings and detailed description.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of cellulose used in the embodiment of the present invention 1 to 3；
Fig. 2 is the transmission electron microscope picture of the nano-cellulose fiber dry powder prepared in the embodiment of the present invention 3；
Fig. 3 is the picture of the nano-cellulose fiber dry powder prepared in the embodiment of the present invention 1 to 4.
Specific embodiment
Embodiment 1-8 preparation parameter is as shown in table 1
1 embodiment 1-8 preparation parameter of table
Embodiment 1-8 according to preparing following preparation method:
1) cellulose/cellulosic material (wood pulp powder, M30 purified cotton, bamboo pulp, straw pulp, reed pulp, filter paper) is taken, wherein
The scanning electron microscope (SEM) photograph of wood pulp powder is as shown in Figure 1, it is seen that cellulose be big fibrous structure, scheme as a comparison, wood pulp powder, bamboo pulp,
Straw pulp, reed pulp, filter paper need to be crushed 200 meshes, be dried to obtain cellulosic material, for use；
2) organic acid (citric acid, ethanedioic acid, malonic acid, maleic acid) is dissolved in alcohol (ethylene glycol, propylene glycol, penta 2
Alcohol, n-octyl alcohol) in, the reaction solution of corresponding 1 volume of table is configured, organic acid mass fraction is shown in Table 1 in reaction solution, in stirring condition
Under, temperature reaction liquid temperature to 1 parameter of table weighs the cellulosic material of 1g, is added in reaction solution, temperature, stirring are kept,
Reaction time is shown in Table 1, until cellulosic material scatters completely；
3) after cellulosic material scatters completely, reaction system is cooled to room temperature, carries out solid-liquid separation treatment by filtering,
Obtain reaction recovered liquid and solid powder, wherein reaction recovered liquid recoverable, the number reused are no more than 6 times, surpass
After crossing 6 times, reaction recovered liquid need to neutralize and be further continued for after distilation using, vapo(u)rizing temperature according to the boiling point of alcohols used into
Row selection.Solid powder is dispersed in ethyl alcohol after ethanol washing, until the mass fraction of solid powder is 0.2%, obtains solid
Powder dispersion liquid；
4) the solid powder dispersion liquid that step 3) obtains is handled through high pressure homogenizer, the pressure that homogenizes be 30000 or
40000psi, processing flow velocity are 30mL/min, obtain nanofiber dispersion liquid；
5) ethyl alcohol being evaporated in step 4) nanofiber dispersion liquid, obtains nano-cellulose fiber dry powder, and photo is shown in Fig. 3,
The transmission electron microscope picture of these nano-cellulose fiber dry powder is as shown in Fig. 2, therefrom it can be clearly seen that nano-cellulose fiber
Diameter within 100nm, length is no less than 300nm.
Redisperse rate of the nano-cellulose fiber dry powder that preparation method of the present invention obtains in pure water is 15-25%, benefit
It is raw material with cellulose-containing material, nano-cellulose fiber dry powder can be prepared with high yield, preparation process whole process is anhydrous, preparation
Organic acid that process uses, alcohol can recycle, and power-product is easier to storage and transport, while also low for the product later period
Cost volume production and application provide good basis.
Claims (10)
1. a kind of preparation method of nano-cellulose fiber dry powder, which is characterized in that have follow steps:
1) cellulose is taken, crushed, be dried to obtain cellulosic material, for use；
2) it takes organic acid and alcohol to mix, obtains reaction solution, the mass fraction of organic acid is 20-30% in reaction solution, and reaction solution adds
The cellulosic material that step 1) obtains, heat preservation, stirring is added to 140-160 DEG C in heat；
3) after cellulosic material is sufficiently destroyed and is dispersed, reaction system carry out solid-liquid separation treatment, obtain reaction recovered liquid and
Solid powder, solid powder are dispersed in alcohol after alcohol washs, and obtain solid powder dispersion liquid；
4) the solid powder dispersion liquid for obtaining step 3) obtains nano-cellulose fiber dispersion liquid through homogenize process；
5) alcohol being evaporated in step 4) nano-cellulose fiber dispersion liquid, obtains nano-cellulose fiber dry powder.
2. the preparation method of nano-cellulose fiber dry powder according to claim 1, it is characterised in that: described in step 1)
Cellulose, selected from rich cellulose-containing plant slurry, it is preferred that select wood pulp or bamboo pulp, be crushed to 200 mesh；Alternatively, step 1)
Described in cellulosic material be purified cotton, the viscosity of purified cotton is not higher than 40mPas.
3. the preparation method of nano-cellulose fiber dry powder according to claim 1, it is characterised in that: described in step 2)
Organic acid is thermal decomposition temperature not less than 160 DEG C and the unitary of alcohol favorable solubility or polynary anhydrous small molecule are sour, described organic
Acid is citric acid, ethanedioic acid, malonic acid, succinic acid, maleic acid, benzene sulfonic acid, monoxone, or acid one kind or more described above
The mixture of kind.
4. the preparation method of nano-cellulose fiber dry powder according to claim 1, it is characterised in that: described in step 2)
Alcohol is the unitary or polynary small molecular alcohol that boiling point is higher than 160 DEG C, and the alcohol is ethylene glycol, propylene glycol, butanediol, n-octyl alcohol, penta
Glycol, or the mixture that alcohol described above is one or more.
5. the preparation method of nano-cellulose fiber dry powder according to claim 1, it is characterised in that: be added in step 2)
The quality and reaction solution volume ratio of cellulosic material are 1g:80-150mL.
6. the preparation method of nano-cellulose fiber dry powder according to claim 1, it is characterised in that: step 2) heating,
In insulating process, keep being condensed back.
7. the preparation method of nano-cellulose fiber dry powder according to claim 1, it is characterised in that: washing in step 3)
It is recycled with alcohol, washing alcohol, dispersion alcohol are not form colloidal dispersions with cellulosic material, can disperse cellulose
Material and boiling point are lower than 100 DEG C of small molecule alcohol, it is preferred that and washing alcohol, dispersion are ethyl alcohol with alcohol, are dispersed in alcohol, point
Scattered solid powder quality and alcohol volume ratio is 1g:450-1000mL.
8. the preparation method of nano-cellulose fiber dry powder according to claim 1, it is characterised in that: described in step 3)
Reaction system carries out solid-liquid separation treatment after being cooled to room temperature.
9. the preparation method of nano-cellulose fiber dry powder according to claim 1, it is characterised in that: described in step 4)
Homogenize process is to handle solid powder dispersion liquid through high pressure homogenizer, and the processing pressure of high pressure homogenizer is 20000-
45000psi, homogenization speed are 30mL/min.
10. a kind of nano-cellulose dry powder, which is characterized in that be made using the preparation method as described in claim 1-9 is any, institute
Diameter≤100nm of nano-cellulose dry powder, length >=200nm are stated, the redisperse rate in pure water is 15-25%.
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Cited By (4)
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| CN110078563A (en) * | 2019-05-31 | 2019-08-02 | 河南农业大学 | Application of the nano-cellulose in terms of rescuing pear tree iron chlorosis disease |
| CN110157393A (en) * | 2019-05-06 | 2019-08-23 | 滨州学院 | Drilling fluid proposes viscous extracting and cutting agent and preparation method with nanofiber-xanthan gum compound |
| CN112694537A (en) * | 2020-12-22 | 2021-04-23 | 佛山(华南)新材料研究院 | Preparation method of oxidized nanocellulose |
| CN115926004A (en) * | 2022-12-27 | 2023-04-07 | 浙江农林大学 | Preparation method of acetyl cellulose citrate |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110157393A (en) * | 2019-05-06 | 2019-08-23 | 滨州学院 | Drilling fluid proposes viscous extracting and cutting agent and preparation method with nanofiber-xanthan gum compound |
| CN110157393B (en) * | 2019-05-06 | 2021-11-16 | 滨州学院 | Nano fiber-xanthan gum compound viscosity-increasing and cutting-extracting agent for drilling fluid and preparation method thereof |
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| CN110078563B (en) * | 2019-05-31 | 2021-10-19 | 河南农业大学 | Application of nano-cellulose in correction of iron deficiency and yellowing disease of pear trees |
| CN112694537A (en) * | 2020-12-22 | 2021-04-23 | 佛山(华南)新材料研究院 | Preparation method of oxidized nanocellulose |
| CN115926004A (en) * | 2022-12-27 | 2023-04-07 | 浙江农林大学 | Preparation method of acetyl cellulose citrate |
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