CN108755215A - A method of preparing nano-cellulose whisker using peanut shell - Google Patents
A method of preparing nano-cellulose whisker using peanut shell Download PDFInfo
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- CN108755215A CN108755215A CN201810422925.3A CN201810422925A CN108755215A CN 108755215 A CN108755215 A CN 108755215A CN 201810422925 A CN201810422925 A CN 201810422925A CN 108755215 A CN108755215 A CN 108755215A
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- peanut shell
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
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Abstract
The invention discloses a kind of methods preparing nano-cellulose whisker using peanut shell, pass sequentially through following steps realization：Discarded peanut shell is first cleaned into dries pulverizing and obtains the peanut shell powder that its grain size is less than 0.2mm, again immersion treatment is carried out with lye and EDTA solution successively, then it is reacted in the mixed liquor of formic acid and hydrogen peroxide and carries out three sections of different temperatures formula digesting technoloy decolorations, use TEMPO oxidizing process acquisition pH value for 7 wet pulp later, it can peanut shell nano-cellulose whisker after being freeze-dried after finally filtering.The method of the present invention has expanded the raw material range for preparing nano-cellulose whisker using discarded peanut shell resource to prepare nano-cellulose whisker, and entire preparation method environmental protection, the degree for removing lignin is higher, and safe, and can also obtain the high cellulose whiskers of crystallinity.
Description
Technical field
The present invention relates to the preparation methods of nano-cellulose whisker.More particularly to a kind of to be prepared using discarded peanut shell
The method of nano-cellulose whisker.
Background technology
With the development of society, resource and environment has become the two big projects for restricting human development, it is renewable, free of contamination
Green new material is both the direction of scientific technological advance, even more the requirement of sustainable development.Cellulose in nature as being distributed
Most extensively, content is most abundant and has the natural macromolecular material of biodegradable, has inexpensive, degradable, friendly to environment
Well, the features such as pollution is not generated.Therefore, the research and development to cellulose are all attached great importance in countries in the world.Plant fiber conduct
The potential advantages of reinforcing material are increasingly paid close attention to by market, compared with inorfil, have that density is small, mechanics and physical
Energy is good, biodegradability is excellent and has the characteristics that recyclability.In addition, lateral dimension can be obtained through sour water solution in cellulose
Within 20nm, the nano-cellulose whisker (CNW) with nanoscale of length about 200nm, intensity and Young's modulus with
General fibre element, which is compared, exponential increase.The Young's modulus of pure CNW is about 150GPa, and tensile strength is about 10GPa, be can use
Generation ceramics and metal have great potential in enhancing polymer composites field.
Currently, the method for preparing Cellulose nanocrystal palpus mainly has acid-hydrolysis method, biological enzyme and physicomechanical processes, wherein
Biological enzyme and physicomechanical processes it is expensive, need special installation etc. due to application it is not extensive；Acid-hydrolysis method uses
It needs to use a large amount of concentrated acids in the process, there are security risk and be easy to cause raw material charing.Oxidizing process makes cellulose molecular chain
Glycosidic bond catalytic cleavage, destroying amorphous region makes cellulose degradation, obtains nano-cellulose whisker.
Existing about 10.74 ten thousand hm of peanut cultivation area in Fujian Province2(statistical data), is mainly distributed on region following the line of the sea, is only
Inferior to the third-largest crop after rice, sweet potato.In recent years, peanut is just expanding year by year because of the higher cultivated area of its economic value,
Planting area also gradually extends, and peanut has become one of the important crops of new round agricultural structure adjustment.And as peanut produces
Amount is continuously improved, and processing and utilization total amount increases, and is always existed in the processing of peanut and ignores the pairs such as its skin, shell depending on its kernel emphatically
The case where product utilization.In addition to being used as roughage on a small quantity, a large amount of peanut shell is burned off or throws away in vain, without adequately and reasonably
It utilizes, wastes resource.Showing research staff as a result, uses different chemical methodes to extract cellulose by raw material of peanut shell, but
A large amount of chlorine-containing compounds and the concentrated sulfuric acid are used in existing chemical method, and preparation method is made to there is peace not environmentally and in preparation process
The problem of full hidden danger.
In view of this, the present inventor furthers investigate the above problem, generated then by this case.
Invention content
It prepares environmentally friendly, safe, efficient the purpose of the present invention is to provide a kind of, and cellulose whiskers crystallinity can be made high
Be prepared by the method that peanut shell prepares nano-cellulose whisker using discarded peanut shell.
To achieve the above object, the present invention uses such technical solution：
A method of nano-cellulose whisker being prepared using peanut shell, is made by the steps：
(1), it will be dried after the clean removal of impurities of discarded peanut shell, crushed after drying and obtain the flower that its grain size is less than 0.2mm
Raw shell powder；
(2), the peanut shell powder of step (1) is poured into the lye that its mass fraction is 1%~10% impregnate it is 4~10 small
When, peanut shell powder is immersed in lye when immersion, is washed with deionized water after immersion and is drained only, its mass fraction is poured into after draining
To be impregnated 4~10 hours in 0.5%~2% EDTA solution, peanut shell powder is immersed in EDTA solution when immersion, Zhi Houyong
Deionized water cleans drying, obtains processing powder；
(3), the processing powder of step (2) is poured into the mixed liquor of formic acid and hydrogen peroxide, 1 is stirred at 20~30 DEG C
~2 hours, be warming up to 40~60 DEG C continue stirring 1~2 hour after filter, after suction filtration add equivalent above-mentioned formic acid and peroxidating
The mixed liquor of hydrogen, and stirred 1~2 hour at 20~30 DEG C, it is washed with deionized water later only to pH=7, finally filters drying
Obtain peanut shell cellulose；
(4), the peanut shell cellulose of step (3) is obtained to the wet pulp of pH=7 using TEMPO oxidizing process；Mistake successively later
Filter, freeze-drying obtain dried object, this dried object is peanut shell nano-cellulose whisker.
Peanut shell is crushed using pulverizer in above-mentioned steps (1), its grain size can be arrived less than 0.2mm's by smashing it through 80 mesh sieve
Peanut shell powder.
Lye in above-mentioned steps (2) is one kind in sodium hydroxide solution and potassium hydroxide solution.
The mixing ratio of above-mentioned formic acid and hydrogen peroxide is 0.5:1,1:1,1:One kind in 0.5, and above-mentioned formic acid and mistake
The processing powder of the mixed liquor submergence above-mentioned steps (2) of hydrogen oxide.
The TEMPO oxidizing process of above-mentioned steps (4) is realized by following steps：
(a) the peanut shell cellulose of above-mentioned steps (3) is added in TEMPO oxidising agents and is dispersed with stirring, TEMPO oxidations
Reagent is by TEMPO, NaBr and NaClO dispersing and dissolving in Na2CO3-NaHCO3Buffer forms, wherein TEMPO, NaBr
Mass ratio with NaClO is 1：5~20:500~1000, per 1g peanut shell celluloses needed for TEMPO oxidising agents be 20~
The dosage of 100mL, TEMPO are the 0.5~2% of peanut shell cellulose quality；
(b), the reaction system of step (a) is placed in thermostat water bath, and is stirred under 20~40 DEG C of steady temperature
Reaction 2~4 hours is added 10~50mL ethyl alcohol and terminates reaction, centrifuges and obtain oxidation slurry at the end of reaction；
(c), the oxidation slurry dilute hydrochloric acid solution of 0.1~1mol/L of step (b) is acidified 0.5~1 hour, and dilute hydrochloric acid
Solution submergence oxidation slurry, is washed with deionized water after acidification to pH=7.
In above-mentioned steps (c), oxidation slurry is stored after deionized water is cleaned at 5-8 DEG C spare.
In above-mentioned steps (4), the filtering of wet pulp uses ultrafiltration membrane or dialysis of its molecular cut off for 8000~14000
Bag filtering.
After adopting the above technical scheme, a kind of method preparing nano-cellulose whisker using peanut shell of the present invention, with
Extraction source of the discarded peanut shell as nano-cellulose whisker, has expanded the raw material range for preparing nano-cellulose whisker,
Be conducive to the raw material sources for accelerating to break through nano-cellulose whisker limitation, realize that nano-cellulose whisker commercially produced product goes out early
Stove, while propose higher value application peanut shell waste resource one opens one's minds；Further more, passing through formic acid and hydrogen peroxide phase
The three-stage boiling mode of cooperation can realize chlorine-free bleaching, operating method environmental protection, and the degree for removing lignin is higher；In addition,
TEMPO oxidizing process is milder, avoids in classical acid method preparation method and there are problems that safe operation using the concentrated sulfuric acid, whole
A safe preparation process, and the high cellulose whiskers of crystallinity can also be obtained.
Description of the drawings
Fig. 1 is peanut husk as raw material and peanut shell nano-cellulose whisker comparison diagram in the present invention；
Wherein：A-peanut shell powder, B-peanut shell nano-cellulose whisker
Fig. 2 is the X-ray diffractogram of peanut shell nano-cellulose whisker prepared by the present invention；
Fig. 3 is the peanut shell nano-cellulose whisker of embodiment one and the peanut shell nano-cellulose whisker of embodiment two
X-ray diffraction comparison diagram.
Wherein：The X-ray diffraction of one peanut shell nano-cellulose whisker of a-embodiment, two peanut shell nanometer of b-embodiment
The X-ray diffraction of cellulose whiskers
Specific implementation mode
In order to further explain the technical solution of the present invention, being explained in detail the present invention below by specific embodiment
It states.
Embodiment one：
A kind of method preparing nano-cellulose whisker using peanut shell of the present invention, embodiment one, as follows
It is prepared：
(1), it will be dried after the clean removal of impurities of discarded peanut shell, crushed using pulverizer after drying, smash it through 80 mesh
Sieve can arrive the peanut shell powder that its grain size is less than 0.2mm, as shown in the A pictures of Fig. 1；
(2), the peanut shell powder of 50 grams of above-mentioned steps (1) is taken to pour into the sodium hydroxide solution that its mass fraction is 5%
It impregnates 5 hours, removes hemicellulose and lignin, sodium hydroxide solution, which should ensure that, when immersion is totally submerged peanut shell powder, soaks
It is washed with deionized water after bubble and drains only, pour into the EDTA solution that its mass fraction is 1% and impregnate 5 hours after draining, removing calcium,
Magnesium ion, EDTA solution, which should ensure that, when immersion is totally submerged peanut shell powder, and net drying is washed with deionized water later, is handled
Powder；
(3), it takes the processing powder of 10 grams of steps (2) to pour into the mixed liquor of 150mL and is obtained by the reaction under mechanical stirring
Reaction system, the necessary Immersion treatment powder of this mixed liquor, mixed liquor is the solution made of formic acid and hydrogen peroxide mixed preparing,
The mixing ratio of formic acid and hydrogen peroxide is 1：1, by reaction system at 25 DEG C heated at constant temperature and stir 1 hour, be warming up to 50
It is filtered after DEG C continuing stirring 1 hour, adds the above-mentioned mixed liquor of 150mL after suction filtration again, and heated at 25 DEG C and continue to stir
It mixes 1 hour, is washed with deionized water later to neutral (pH value for being washed to whole system with deionized water is 7), is finally filtered
Powdery is dried and is ground into, this powder is peanut shell cellulose；
(4), the peanut shell cellulose of 10 grams of steps (3) is taken to obtain the wet pulp of pH=7 using TEMPO oxidizing process；Specific behaviour
Work is that 0.0125g TEMPO, 0.125g NaBr and 12.5g NaClO is taken to be dissolved in Na2CO3-NaHCO3It is prepared in buffer solution
TEMPO oxidising agents, this Na2CO3-NaHCO3The additive amount of buffer solution is that TEMPO oxidising agents is made to reach 1000ml, and 10g is spent
Raw case fibre element, which is added in 1000mL TEMPO oxidising agents, to be dispersed with stirring, and constant temperature stirs in 25 DEG C of thermostat water bath later
It mixes, is stirred to react 4 hours, 20mL ethyl alcohol is added at the end of reaction and terminates reaction, is centrifuged with centrifugal separator after terminating reaction
Oxidation slurry is obtained, oxidation slurry dilute hydrochloric acid solution is acidified 30min, and effect is to convert the carboxylic acid sodium salt in oxidized fibre to carboxylic
Then acid is washed with deionized to obtain the wet pulp of pH=7, this wet pulp is stored spare at 5-8 DEG C；In this step, Na2CO3-
NaHCO3The dosage of buffer solution is to make the TEMPO oxidising agents needed for every 1 gram of peanut shell cellulose be 20~100mL, and TEMPO
Dosage be peanut shell cellulose quality 0.5~2%, in this way, peanut shell cellulose dosage determine after TEMPO dosages and
The dosage of TEMPO oxidising agents accordingly determines that the dosage of NaBr and NaClO accordingly determines after TEMPO dosages determine, finally
Na2CO3-NaHCO3The dosage of buffer solution is also determined；
(5), the wet pulp of step (4) is filtered using bag filter, specifically：It will be packed into its section after wet pulp centrifugal concentrating
Stay dialysis in the bag filter that molecular weight is 8000~14000 (bag filter need to be handled first and be reused, and the processing mode of bag filter is,
Bag filter is cut into the segment of 10cm long, the segment being cut into later, which is put into boiling water, to be boiled 5 minutes, then just may be used after being cleaned with distilled water
Using), dialysis time is 72 hours, dialysis initial stage using magnetic stirrer 4 hours to accelerate to dialyse, in dialysis procedure often
A water is changed within 12 hours, and it is 7 to control dialyzate pH value；Finally the suspension that dialysis obtains is cleaned in ultrasonic cleaner
10min, water temperature are controlled at 25 DEG C, finely dispersed peanut shell Cellulose nanocrystal palpus suspended emulsion are obtained, by peanut shell cellulose
Nano whisker suspended emulsion is freeze-dried 1h under the conditions of -10 DEG C, obtains dried object, this dried object is peanut shell Cellulose nanocrystal
Must, as shown in the B pictures of Fig. 1.
Peanut shell Cellulose nanocrystal palpus obtained with the aforedescribed process is adopted, as shown in Figure 2, it can be seen that fiber obtained
The diffraction maximum of plain whisker is between 2 θ=13-23 °, and high and sharp, crystal surface area is big, this shows the fiber extracted from peanut shell
Plain whisker has higher crystallinity, is to show apparent diffraction maximum at about 16.5 ° and 22.6 ° two in 2 θ, they are respectively
(110) the diffractive features peak of crystal face and (002) crystal face, the structure are typical cellulose I type crystal form, the knot of the cellulose whiskers
Brilliant degree is calculated according to Segal methods, and the content of crystalline region and amorphous area in cellulose whiskers is represented with the intensity of (002) crystal face, and
(110) intensity of crystal face represents the content of amorphous area in cellulose whiskers, calculate the crystallinity of the cellulose whiskers is
70.1%.This illustrates that the starch of script, lignin etc. are eliminated in preparation process in cellulose, and fine in preparation process
The crystal structure of dimension element is not destroyed.
A kind of method preparing nano-cellulose whisker using peanut shell of the present invention, has the advantages that, with useless
Extraction source of the peanut shell abandoned as nano-cellulose whisker, has expanded the raw material range for preparing nano-cellulose whisker, has had
Limit to conducive to the raw material sources for accelerating to break through nano-cellulose whisker, realizes that nano-cellulose whisker commercially produced product goes out early
Stove, while propose higher value application peanut shell waste resource one opens one's minds；Further more, people studies to obtain through the invention
Formic acid and the matched three-stage boiling mode of hydrogen peroxide can realize chlorine-free bleaching, operating method environmental protection, and removing wooden
The degree of element is higher；In addition, TEMPO oxidizing process is milder, avoids in traditional preparation methods and existed using a large amount of concentrated sulfuric acids
The problem of safe operation, whole preparation process safety, and the cellulose whiskers that crystallinity is high, major diameter is big can also be obtained.
Embodiment two：
A kind of method preparing nano-cellulose whisker using peanut shell of the present invention, embodiment two, as follows
It is prepared：
(1) it will dry after the clean removal of impurities of discarded peanut shell, crushed using pulverizer after drying, smash it through 80 mesh sieve
The peanut shell powder that its grain size is less than 0.2mm can be arrived；
(2) it takes the peanut shell powder of 50 grams of above-mentioned steps (1) to pour into the sodium hydroxide solution that its mass fraction is 7% to soak
Bubble 8 hours, removes hemicellulose and lignin, and sodium hydroxide solution should be totally submerged peanut shell powder when immersion, be used after immersion
Deionized water clean drains, poured into after draining its mass fraction be 2% EDTA solution in impregnates 8 hours, removing calcium, magnesium from
Son, EDTA solution should be totally submerged peanut shell powder when immersion, and net drying is washed with deionized water later, obtain processing powder；
(3) it takes the processing powder of 10 grams of steps (2) to pour into the mixed liquor of 150mL and is obtained by the reaction under mechanical stirring anti-
Answer system, mixed liquor is the solution made of formic acid and hydrogen peroxide mixed preparing, and the mixing ratio of formic acid and hydrogen peroxide is
2：1, by reaction system at 30 DEG C heated at constant temperature and stir 1 hour, be warming up to 60 DEG C continue stirring 1 hour after filter, filter
It adds the above-mentioned mixed liquor of 150mL again afterwards, and stirring 2 hours is heated and continued at 30 DEG C, be washed with deionized water later net
To neutrality, finally filters dry and be ground into powdery, this powder is peanut shell cellulose；
(4) take the peanut shell cellulose of 10 grams of steps (3) that TEMPO oxidizing process is used to obtain pH value as 7 wet pulp；Specific behaviour
Work is that 0.025g TEMPO, 0.25g NaBr and 25g NaClO are dissolved in Na2CO3-NaHCO3TEMPO is prepared in buffer solution
Oxidising agent, this Na2CO3-NaHCO3The additive amount of buffer solution is that TEMPO oxidising agents is made to reach 1000ml, by 10g peanut shells
Cellulose is added in 1000mL TEMPO oxidising agents and is dispersed with stirring, and is placed in constant temperature in 30 DEG C of thermostat water bath and stirs, stirring
Reaction 5 hours is added 20mL ethyl alcohol and terminates reaction, aoxidized with centrifugal separator to centrifuge after terminating reaction at the end of reaction
Slurry, oxidation slurry dilute hydrochloric acid solution are acidified 30min, and effect is to convert the carboxylic acid sodium salt in oxidized fibre to carboxylic acid, then
It is washed with deionized to obtain the wet pulp that pH value is 7, this wet pulp is stored spare at 5-8 DEG C；
(5) it uses its molecular cut off to be filtered for 8000~14000 ultrafiltration membrane the wet pulp of step (4), filters
Filter residue afterwards is freeze-dried 1h under the conditions of -10 DEG C, obtains dried object, this dried object is peanut shell Cellulose nanocrystal palpus.
Peanut shell nano-cellulose whisker made from embodiment three is scanned using X-ray scanners, crystallization is special
It is with the XRD diagram of peanut shell nano-cellulose whisker of embodiment one, two close to levy peak, and is computed it can be seen that embodiment three
The crystallinity of peanut shell nano-cellulose whisker is up to 65%.
The mode of above-described embodiment and the non-limiting present invention, any person of an ordinary skill in the technical field do it
Appropriate changes or modifications, all should be regarded as not departing from the patent category of the present invention.
Claims (7)
1. a kind of method preparing nano-cellulose whisker using peanut shell, which is characterized in that be made by the steps：
(1), it will be dried after the clean removal of impurities of discarded peanut shell, crushed after drying and obtain the peanut shell that its grain size is less than 0.2mm
Powder；
(2), the peanut shell powder of step (1) is poured into the lye that its mass fraction is 1%~10% and is impregnated 4~10 hours,
Peanut shell powder is immersed in lye when immersion, is washed with deionized water after immersion and is drained only, its mass fraction is poured into after draining and is
It is impregnated 4~10 hours in 0.5%~2% EDTA solution, peanut shell powder is immersed in EDTA solution when immersion, is spent later
Ionized water cleans drying, obtains processing powder；
(3), the processing powder of step (2) is poured into the mixed liquor of formic acid and hydrogen peroxide, 1~2 is stirred at 20~30 DEG C
Hour, be warming up to 40~60 DEG C continue stirring 1~2 hour after filter, after suction filtration add equivalent above-mentioned formic acid and hydrogen peroxide
Mixed liquor, and stir 1~2 hour, be washed with deionized water later only to pH=7 at 20~30 DEG C, finally filter dry
To peanut shell cellulose；
(4), the peanut shell cellulose of step (3) is obtained to the wet pulp of pH=7 using TEMPO oxidizing process；It filters successively later, is cold
Freeze drying to obtain dried object, this dried object is peanut shell nano-cellulose whisker.
2. a kind of method preparing nano-cellulose whisker using peanut shell according to claim 1, it is characterised in that：On
It states peanut shell in step (1) to crush using pulverizer, the peanut shell powder that its grain size is less than 0.2mm can be arrived by smashing it through 80 mesh sieve
End.
3. a kind of method preparing nano-cellulose whisker using peanut shell according to claim 1, it is characterised in that：On
It is one kind in sodium hydroxide solution and potassium hydroxide solution to state the lye in step (2).
4. a kind of method preparing nano-cellulose whisker using peanut shell according to claim 1, it is characterised in that：On
The mixing ratio for stating formic acid and hydrogen peroxide is 0.5:1,1:1,1:One kind in 0.5, and above-mentioned formic acid and hydrogen peroxide is mixed
Close the processing powder of liquid submergence above-mentioned steps (2).
5. a kind of method preparing nano-cellulose whisker using peanut shell according to claim 1, it is characterised in that：On
The TEMPO oxidizing process for stating step (4) is realized by following steps：
(a) the peanut shell cellulose of above-mentioned steps (3) is added in TEMPO oxidising agents and is dispersed with stirring, TEMPO oxidising agents
It is by TEMPO, NaBr and NaClO dispersing and dissolving in Na2CO3-NaHCO3Buffer forms, wherein TEMPO, NaBr and
The mass ratio of NaClO is 1：5~20:500~1000, per 1g peanut shell celluloses needed for TEMPO oxidising agents be 20~
The dosage of 100mL, TEMPO are the 0.5~2% of peanut shell cellulose quality；
(b), the reaction system of step (a) is placed in thermostat water bath, and 2 is stirred to react under 20~40 DEG C of steady temperature
~4 hours, 10~50mL ethyl alcohol is added at the end of reaction and terminates reaction, centrifuges and obtains oxidation slurry；
(c), the oxidation slurry dilute hydrochloric acid solution of 0.1~1mol/L of step (b) is acidified 0.5~1 hour, and dilute hydrochloric acid solution
Submergence oxidation slurry, is washed with deionized water after acidification to pH=7.
6. a kind of method preparing nano-cellulose whisker using peanut shell according to claim 5, it is characterised in that：?
In above-mentioned steps (c), oxidation slurry is stored after deionized water is cleaned at 5-8 DEG C spare.
7. a kind of method preparing nano-cellulose whisker using peanut shell according to claim 1, it is characterised in that：On
It states in step (4), the filtering of wet pulp uses its molecular cut off to be filtered for 8000~14000 ultrafiltration membrane or bag filter.
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| WO2020151282A1 (en) * | 2019-01-25 | 2020-07-30 | 华南理工大学 | Nanocellulose-based refill ink and preparation method therefor |
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| CN103031356A (en) * | 2012-12-19 | 2013-04-10 | 青岛农业大学 | Method for applying peanut shells to synchronously prepare nanocellulose crystal and sugar |
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| CN103031356A (en) * | 2012-12-19 | 2013-04-10 | 青岛农业大学 | Method for applying peanut shells to synchronously prepare nanocellulose crystal and sugar |
| CN104762845A (en) * | 2015-04-13 | 2015-07-08 | 东华大学 | Method for extracting cellulose nanowhiskers from corn husks |
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| WO2020151282A1 (en) * | 2019-01-25 | 2020-07-30 | 华南理工大学 | Nanocellulose-based refill ink and preparation method therefor |
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