CN110183538A - A kind of method of the slightly sour preparation Cellulose nanocrystal body of promotion system altogether of inorganic fused salt- - Google Patents
A kind of method of the slightly sour preparation Cellulose nanocrystal body of promotion system altogether of inorganic fused salt- Download PDFInfo
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- CN110183538A CN110183538A CN201910544934.4A CN201910544934A CN110183538A CN 110183538 A CN110183538 A CN 110183538A CN 201910544934 A CN201910544934 A CN 201910544934A CN 110183538 A CN110183538 A CN 110183538A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
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Abstract
The invention discloses a kind of methods of the slightly sour preparation Cellulose nanocrystal body of promotion system altogether of inorganic fused salt -: cellulose-containing raw material is added in the slightly sour promotion system altogether of inorganic fused salt -, it is warming up to 50 DEG C -130 DEG C, persistently stir 0.5-72 hours, obtain uniform system, then it dialyses by desalination, Cellulose nanocrystal body aqueous solution is obtained, Cellulose nanocrystal body is obtained after freeze-dried, the inorganic fused salt of desalination dialysis abjection continues reuse.The advantage of the invention is that the slightly sour promotion system altogether of inorganic fused salt-has many advantages, such as that environmental-friendly, cheap, easily prepared, formic acid dosage is few, the recyclable recycling of inorganic fused salt.Reaction condition is relatively mild, to equipment corrode it is small and easy to operate, product yield is high.Cellulose nanocrystal body yield obtained is higher, is in corynebacterium structure, has excellent mechanical strength, have broad application prospects in fields such as nanocomposites.
Description
Technical field
The invention belongs to cellulose technology fields, and in particular to a kind of to be prepared using the slightly sour promotion system altogether of inorganic fused salt-
The method of Cellulose nanocrystal body.
Background technique
Cellulose is the most abundant renewable natural resources on the earth, about 180,000,000,000 tons of annual output.In recent years, from various fibres
It ties up extraction nano-cellulose in plain raw material and has become research hotspot both domestic and external.Cellulose nanocrystal body (CNC) is to pass through chemistry
Or cellulosic material is decomposed into the product with nano-scale structure by mechanical means, obtained Cellulose nanocrystal body not only has
There is the inherent characteristic of native cellulose, also there is low-density, high-specific surface area, high-aspect-ratio, biodegradable, high intensity etc.
Excellent characteristic.Therefore, Cellulose nanocrystal body all has wide in fields such as biological medicine, packaging, printing, food industry
Application prospect.
The preparation process of Cellulose nanocrystal body mainly includes acid-hydrolysis method, ionic liquid, eutectic solvent method and machine
Tool method.Wherein, acid-hydrolysis method is the current preparation most common method of Cellulose nanocrystal body, the CNC that acid-hydrolysis method is prepared
Suspension stability with higher, but reaction process is not easy to control, and larger to the corrosion of equipment, is also easy to produce in subsequent processing
A large amount of spent acid and impurity, environmental pollution are larger.In addition, ionic liquid is made by hydrogen bond between destroying cellulosic molecule
CNC, although the solvability of ionic liquid is high, its higher cost and itself is degradable constrains its industrialization promotion.It is low
Congruent melting solvent mainly has quaternary ammonium salt, choline etc. as a kind of novel green solvent, there is steam to force down, is non-toxic, can
The unique physicochemical properties such as biodegrade, strong solubility, the CNC prepared by the solvent have that yield is high, partial size is smaller and
Uniform feature, but quaternary ammonium salt eutectic solvent, under conditions of highly basic and heating, Yi Fasheng hofmann elimination generates
A large amount of by-products；And choline eutectic solvent has certain dissolubility to metal oxide, easily causes consersion unit to corrode, mesh
It is preceding still in the exploratory stage.And Mechanical Method is usually to make hydrogen between fiber by carrying out high shear processing to cellulosic material
Key fracture, Cellulose nanocrystal body is obtained after multiple circular treatment, generallys use high pressure homogenization method, ball-milling method, Ultrasonic Pulverization
Method, but have the shortcomings that energy consumption is high, CNC obtained is easy to reunite, it is unfavorable for industrializing.It is continuous with CNC industrial process as a result,
It promotes, develops a kind of even anacidity environmental protection of nontoxic, few acid and be recycled system and prepare CNC and have become a kind of inevitable trend.
Summary of the invention
The present invention is to solving many equipment burn into systems caused by strong acid in Cellulose nanocrystal body (CNC) preparation process
Problem standby and that environmental protection is at high cost, to accelerate CNC industrialized production process.Using the slightly sour promotion system preparation altogether of inorganic fused salt-
CNC not only can corrode plant issue to avoid current CNC preparation process strong acid, can also realize system recycled for multiple times, drop
Low in acidity Non-aqueous processing difficulty.
The object of the present invention is to provide a kind of sides of the slightly sour preparation Cellulose nanocrystal body of promotion system altogether of inorganic fused salt-
Cellulose nanocrystal body, institute is made after dissociating cellulose amorphous region by the slightly sour total promotion system of inorganic fused salt-in method
Cellulose nanocrystal body obtained has the characteristics that yield is high, crystallinity is high, partial size is small and even size distribution.
Technical scheme is as follows:
A kind of method of the slightly sour preparation Cellulose nanocrystal body of promotion system altogether of inorganic fused salt-, the method includes the steps:
Cellulose-containing raw material is added in the slightly sour promotion system altogether of inorganic fused salt -, 50 DEG C -130 DEG C is warming up to, persistently stirs 0.5-
72 hours, uniform system is obtained, is then dialysed by desalination, Cellulose nanocrystal body aqueous solution is obtained, is obtained after freeze-dried
To Cellulose nanocrystal body；
The solid-liquid mass ratio of the cellulose-containing raw material and the slightly sour promotion system altogether of inorganic fused salt-is 1:10-1:1000.
Preferably, the inorganic fused salt-it is slightly sour altogether promotion system the preparation method comprises the following steps: inorganic fused salt hydrate is dissolved in water
In, inorganic fused salt aqueous solution is obtained, then micro acid is added in above-mentioned inorganic fused salt aqueous solution, it is micro- to obtain inorganic fused salt-
The total promotion system of acid.
Preferably, the inorganic fused salt-is slightly sour is total to the halide that inorganic fused salt hydrate in promotion system is Li, Zn, Ca
(such as LiCl, LiBr, LiI, ZnCl2、ZnBr2、CaCl2、CaBr2Deng), the nitrate (such as Zn (NO of Zn, Li, Ca3)2、LiNO3、
Ca(NO3)2), perchlorate (such as LiClO of Li, Zn, Ca4、Zn(ClO4)2、Ca(ClO4)2) one or more of mixing,
Group becomes single or mixed molten salt system.
Preferably, the mass fraction of inorganic fused salt hydrate is 20- in the slightly sour promotion system altogether of the inorganic fused salt-
80%.
Preferably, the acid in the slightly sour promotion system altogether of the inorganic fused salt-includes inorganic acid (such as: hydrochloric acid, sulfuric acid, nitric acid)
With organic acid (such as: formic acid, acetic acid, carbonic acid).Sour content is 10mM-10M in the slightly sour promotion system altogether of the inorganic fused salt-.
Preferably, the cellulose-containing raw material can be wastepaper (such as Mixed Office WasteMOW), cotton pulp (such as degreasing
Cotton), microcrystalline cellulose, paper pulp (including China paper pulp and pulp inlet).
Preferably, the inorganic fused salt of desalination dialysis abjection continues reuse, can recycle reuse.
Preferably, it is gained after dialyzate is concentrated by evaporation that the inorganic fused salt, which continues reuse, and it is micro- to be back to use inorganic fused salt-
The total promotion system preparation process of acid.
The advantage of the invention is that inorganic fused salt-it is slightly sour altogether promotion system have it is environmental-friendly, cheap, easily prepared,
The advantages that acid adding amount is few, recycling can be recycled in inorganic fused salt.Reaction condition is relatively mild, small to equipment corrosion, and operates letter
Just, product yield is high.After the slightly sour processing of promotion system altogether of inorganic fused salt-, the amorphous region of cellulose is destroyed, cellulose point
Hydrogen bond between son is broken, so that cellulose macromolecule is gradually broken into Cellulose nanocrystal body, and this process reaction item
Part is easy to control, and is avoided cellulose and is acutely damaged.Therefore, the Cellulose nanocrystal body yield of the method preparation is higher, is in
Corynebacterium structure has excellent mechanical strength, has broad application prospects in fields such as nanocomposites.
Detailed description of the invention
Fig. 1 is Cellulose nanocrystal swept-volume electron microscopic picture obtained in the embodiment of the present invention 1.
Fig. 2 is Cellulose nanocrystal body transmission electron microscope picture obtained in the embodiment of the present invention 1.
Specific embodiment
Below with reference to several specific embodiments, the present invention is further elaborated.But these embodiments are only used for
The protection scope that the bright present invention is not intended to limit the present invention.Manufacturer is not specified in agents useful for same or equipment, is accordingly to be regarded as to lead to
Cross the conventional products of market purchase.
Microcrystalline cellulose used in following embodiment is purchased from Sinopharm Chemical Reagent Co., Ltd.'s (column chromatography
(Shanghai examination), CAS:9004-34-6)；Absorbent cotton is purchased from Xu Wei hygienic material Co., Ltd；Mixed Office WasteMOW is collected from office
Room waste paper；Paper pulp is the wealthy slurry of import Russia cloth, after dry pulp plate impregnates 12 hours in deionized water, is discongested with solution is discongested
It is spare to be placed on shady place constant humidity.
Embodiment 1
It is accurate to prepare 100g containing 35%LiBr and LiBr-HCl that content of hydrochloric acid is 0.1M is total to promotion system.Accurately weigh 5g
Microcrystalline cellulose, solid-to-liquid ratio 1:20 are added to LiBr-HCl and are total in promotion system, be warming up to 70 DEG C, persistently stir 12 hours
After obtain uniform system, then carry out desalination dialysis, obtain Cellulose nanocrystal body aqueous solution, obtain fiber after freeze-dried
Plain nanocrystal.Cellulose nanocrystal body yield made from the method is 57%, crystallinity 87%.By scanning electron microscope
Fig. 1 observation is it is found that Cellulose nanocrystal body made from the method is in corynebacterium.Observed by transmission electron microscope figure 2 it is found that this
The average length of Cellulose nanocrystal body made from method is 143nm, average diameter 10nm.
Embodiment 2
The accurate LiCl-H for preparing 200g and being 0.01M containing 60%LiCl and sulfuric acid content2SO4Promotion system altogether.It accurately weighs
1g absorbent cotton, solid-to-liquid ratio 1:200, is added to LiCl-H2SO4Altogether in promotion system, 85 DEG C are warming up to, after persistently stirring 8 hours
To uniform system, desalination dialysis is then carried out, Cellulose nanocrystal body aqueous solution is obtained, obtains cellulose after freeze-dried and receive
Meter Jing Ti.Cellulose nanocrystal body yield made from the method is 64%, crystallinity 82%, and average length 131nm is average
Diameter is 13nm, is in corynebacterium.
Embodiment 3
The accurate 100g for preparing contains 55%CaCl2And formic acid content is the CaCl of 4M2Formic acid is total to promotion system.Accurately weigh 1g
Paper pulp, solid-to-liquid ratio 1:100, is added to CaCl2Formic acid is total in promotion system, is warming up to 110 DEG C, after persistently stirring 7 hours
To uniform system, desalination dialysis is then carried out, Cellulose nanocrystal body aqueous solution is obtained, obtains cellulose after freeze-dried and receive
Meter Jing Ti.Cellulose nanocrystal body yield made from the method is 61%, crystallinity 79%, and average length 137nm is average
Diameter is 15nm, is in corynebacterium.
Embodiment 4
Cellulose nanocrystal body is prepared by raw material of Mixed Office WasteMOW, waste paper is crushed, crosses 40-60 mesh.Firstly, quasi-
It really prepares 150g and contains 70%LiClO4And sulfuric acid content is the LiClO of 1M4-H2SO4Promotion system altogether.Accurately weigh 0.2g crushing
Waste paper afterwards, solid-to-liquid ratio 1:750, is added to LiClO4-H2SO4Altogether in promotion system, 100 DEG C are warming up to, it is small persistently to stir 18
When after obtain uniform system, then carry out desalination dialysis, obtain Cellulose nanocrystal body aqueous solution, obtain fibre after freeze-dried
Tie up plain nanocrystal.Cellulose nanocrystal body yield made from the method is 57%, crystallinity 84%, and average length is
156nm, average diameter 11nm are in corynebacterium.
5 cycle example of embodiment
With during the Cellulose nanocrystal body that is prepared in embodiment 2, resulting recycling after being concentrated by evaporation by dialyzate
LiCl be inorganic fused salt, prepare 100g containing 60%LiCl and LiCl- formic acid that formic acid content is 1M be total to promotion system.It is accurate to claim
0.1g microcrystalline cellulose is taken, solid-to-liquid ratio 1:1000 is added to LiCl- formic acid and is total to promotion system, is warming up to 110 DEG C, persistently stirs
Uniform system is obtained after mixing 15 hours, desalination dialysis is then carried out, Cellulose nanocrystal body aqueous solution is obtained, after freeze-dried
Obtain Cellulose nanocrystal body.Cellulose nanocrystal body yield made from the method is 67%, crystallinity 83%, average length
It is in corynebacterium for 128nm, average diameter 13nm.
For any person skilled in the art, without departing from the scope of the technical proposal of the invention, all
Many possible changes and modifications are made to technical solution of the present invention using the technology contents of the disclosure above, or are revised as equivalent
The equivalent embodiment of variation.Therefore, anything that does not depart from the technical scheme of the invention, according to the technical essence of the invention to
Any simple modifications, equivalents, and modifications that upper embodiment is done should all still fall within the range of technical solution of the present invention protection
It is interior.
Claims (10)
1. a kind of method of the slightly sour preparation Cellulose nanocrystal body of promotion system altogether of inorganic fused salt-, which is characterized in that the method
Comprising steps of
Cellulose-containing raw material is added in the slightly sour promotion system altogether of inorganic fused salt -, is warming up to 50 DEG C -130 DEG C, it is lasting to stir
It 0.5-72 hours, dialyses using desalination, obtains Cellulose nanocrystal body aqueous solution, cellulose nanometer is obtained after freeze-dried
Crystal；
The solid-liquid mass ratio of the cellulose-containing raw material and the slightly sour promotion system altogether of inorganic fused salt-is 1:10-1:1000.
2. the method for the slightly sour preparation Cellulose nanocrystal body of promotion system altogether of inorganic fused salt-according to claim 1, special
Sign is that the inorganic fused salt hydrate in the slightly sour promotion system altogether of the inorganic fused salt-is halide, the nitric acid of Li, Zn, Ca
The mixing of one or more of salt, perchlorate.
3. the method for the slightly sour preparation Cellulose nanocrystal body of promotion system altogether of inorganic fused salt-according to claim 1, special
Sign is that the mass fraction of inorganic fused salt hydrate is 20-80% in the slightly sour promotion system altogether of the inorganic fused salt-.
4. the method for the slightly sour preparation Cellulose nanocrystal body of promotion system altogether of inorganic fused salt-according to claim 1, special
Sign is that the acid in the slightly sour promotion system altogether of the inorganic fused salt-is inorganic acid or organic acid.
5. the method for the slightly sour preparation Cellulose nanocrystal body of promotion system altogether of inorganic fused salt-according to claim 4, special
Sign is that the inorganic acid is hydrochloric acid, sulfuric acid or nitric acid；The organic acid is formic acid, acetic acid or carbonic acid.
6. the method for the slightly sour preparation Cellulose nanocrystal body of promotion system altogether of inorganic fused salt-according to claim 1, special
Sign is that sour content is 10mM-10M in the slightly sour promotion system altogether of the inorganic fused salt-.
7. the method for the slightly sour preparation Cellulose nanocrystal body of promotion system altogether of inorganic fused salt-according to claim 1, special
Sign is that the cellulose-containing raw material is one or more of microcrystalline cellulose, cotton pulp, paper pulp, wastepaper.
8. the method for the slightly sour preparation Cellulose nanocrystal body of promotion system altogether of inorganic fused salt-according to claim 1, special
Sign is that the inorganic fused salt of the desalination dialysis abjection continues reuse.
9. the method for the slightly sour preparation Cellulose nanocrystal body of promotion system altogether of inorganic fused salt-according to claim 8, special
Sign is that it is gained after dialyzate is concentrated by evaporation that the inorganic fused salt, which continues reuse, and is back to use the slightly sour total promotion of inorganic fused salt-
In system.
10. a kind of method of the slightly sour preparation Cellulose nanocrystal body of promotion system altogether of inorganic fused salt-, which is characterized in that pass through power
Benefit requires method described in any one of 1-9 to be prepared.
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| CN114805615A (en) * | 2022-03-24 | 2022-07-29 | 华南农业大学 | Method for preparing cellulose nanocrystal by hydrolyzing acidic zinc chloride, cellulose nanocrystal prepared by method and application of cellulose nanocrystal |
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Application publication date: 20190830 |