CN109338781A - A kind of steam blasting combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose - Google Patents
A kind of steam blasting combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose Download PDFInfo
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- CN109338781A CN109338781A CN201811191962.4A CN201811191962A CN109338781A CN 109338781 A CN109338781 A CN 109338781A CN 201811191962 A CN201811191962 A CN 201811191962A CN 109338781 A CN109338781 A CN 109338781A
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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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- 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
- D21C5/005—Treatment of cellulose-containing material with microorganisms or enzymes
Abstract
The invention belongs to biomass nano Material Fields, are related to a kind of method for preparing nano-cellulose, combine the high-pressure homogeneous method for preparing nano-cellulose using steam blasting using peanut shell as raw material more particularly, to a kind of.Nano-cellulose is made by steam blasting, chlorite bleaching, enzymolysis processing, high-pressure homogeneous, centrifugation and freezing dry process in method of the invention.Preparation is simple by the present invention, and chemicals usage is few, and yield is high, is suitable for large-scale industrialized production, the nano-cellulose particle diameter distribution of preparation is uniform, draw ratio is big, crystallinity is high.The present invention makes full use of the thermomechanical chemical effect of steam blasting, effective to remove most of hemicellulose and lignin, is acted on using high-pressure homogeneous high pressure and Strong shear, efficiently, quickly prepares nanofiber.
Description
Technical field
The invention belongs to biomass nano Material Fields, are related to a kind of method for preparing nano-cellulose, especially
Be related to it is a kind of using peanut shell as raw material using steam blasting combine the high-pressure homogeneous method for preparing nano-cellulose.
Background technique
Nano-cellulose is to remove the crystal region of amorphous region and low-crystallinity in cellulose, and extraction obtains one kind and receives
The cellulose crystallite body of meter-sized (1-100nm).It has excellent mechanical performance, huge specific surface area, high-crystallinity,
High-hydrophilic, the high grade of transparency, low-density, good biodegradability and biocompatibility and stable chemical property, can
It is widely used in the fields such as bio-pharmaceuticals, food processing, functional material, cosmetics and papermaking.
Peanut is one of big oil crops in China three, and peanut shell is as the by-product in process, every year about 500
Ten thousand tons of yield.At present except on a small quantity be used as feed in addition to, most of peanut shell is simply discarded or burns, cause the wasting of resources and
Environmental pollution.Peanut shell contains a large amount of cellulose, prepares nano-cellulose using peanut shell, not only low in raw material price, can
High-cost cotton, flax etc. are substituted, and is conducive to the deep processing of agricultural and sideline product and the processing of waste, brings huge warp
It can reduce environmental pollution while benefit of helping, open up new approach for the comprehensive utilization of peanut.
The preparation of nano-cellulose at present mainly uses acid-hydrolysis method, but the method can consume a large amount of acid and water, and chemistry is dirty
Dye is serious, higher cost.Steam explosion technology is a kind of physical method of separating plant fiber developed in recent years, is had
The advantages that high efficiency, low cost, pollution-free, short processing time, chemicals usage are few.Cellulosic material is after steam blasting, knot
Structure is fluffy, and molecular degradation is easily removed hemicellulose and lignin.High-pressure homogeneous is a kind of with mechanical force and fuel factor
Physical method, the high-velocity fluid that is formed can achieve Nano grade after Strong shear, high pressure processing.However steam blasting
It is also rarely reported in conjunction with the high-pressure homogeneous method for preparing peanut shell nano-cellulose.
Summary of the invention
In order to solve the above technical problems, steam blasting and high-pressure homogeneous heat are made full use of the present invention provides a kind of
The method of mechanochemical effect acquisition peanut shell nano-cellulose；Prepared peanut shell nanofiber by means of the present invention
Element few, short processing time using chemical reagent, mechanical performance and biocompatibility are excellent.
It is by following technologies that steam blasting of the present invention, which combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose,
Scheme is come the technical problem more than solving:
A kind of steam blasting combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose, includes the following steps:
(1) pre-process: cleaning peanut husk as raw material is dried, is crushed, and sieving obtains peanut shell powder；
(2) steam blasting: being added water in the peanut shell powder in (1), and after swollen 6-12h then steam blasting uses hot water
It washs and filters, obtain a filter residue；
(3) chlorite bleaching: a filter residue in (2) is placed in reaction kettle, adjusts pH4-5, and NaClO is added2, permanent
Tepidarium, stirring filter after washing to neutrality, obtain secondary filter residue；
(4) enzymolysis processing: being made into aqueous dispersions for peanut case fibre obtained by (3), and cellulase, enzymatic hydrolysis, enzyme deactivation is added；
(5) high-pressure homogeneous: by peanut shell fiber enzymolysis liquid ultrasonic disperse obtained by (4), then homogeneous；
(6) it is centrifuged, is freeze-dried: the solution of (5) mesohigh homogeneous is centrifuged, collect supernatant, supernatant is freezed dry
It is dry, obtain peanut shell nano-cellulose powder.
Specific steps are as follows:
(1) it pre-processes: peanut husk as raw material being spent into ionized water cleaning, is dried, is crushed, sieve with 100 mesh sieve；
(2) steam blasting: being added water in the peanut shell powder in (1), makes water content 5-40wt%, swollen 6-12h
It is placed on steam explosion chamber, steam blasting pressure is set as 0.5-3.0MPa, explosion 20-100s, uses 50-70 DEG C of hot water wash after explosion treatment
It washs and filters, obtain a filter residue；
(3) filter residue of gained and deionized water in step (2) chlorite bleaching: are pressed into feed liquid mass volume ratio 1g:
20mL is placed in reaction kettle, is 4-5 using acetic acid adjustment pH value of solution, the NaClO of 15g/L is added2, the thermostatted water at 40-60 DEG C
Bath stirs 3-6h, will filter after residue washing to neutrality, obtain secondary filter residue；
(4) enzymolysis processing: the citrate-phosphate disodium hydrogen buffer solution for being 4-6 with pH is by secondary filter residue obtained by step (3)
The aqueous dispersions of 0.5-10wt% are configured to, cellulase is added, the dosage of cellulase is 400-5000U/g, is placed in 40-50
4-6h, then 80 DEG C of water-bath 30-40min enzyme deactivations are stirred in water bath with thermostatic control at DEG C；
(5) high-pressure homogeneous: by the first ultrasonic disperse 5- under the power of 200W of peanut shell fiber enzymolysis liquid obtained by step (4)
10min, supersonic frequency 20kHz, then homogeneous 3-6 times under the pressure of 400-800bar；
(6) it is centrifuged, is freeze-dried: the high-pressure homogeneous solution of step (5) is centrifuged 5-15min through 10000r/min, collect
Supernatant is freeze-dried up to peanut shell nano-cellulose powder by supernatant.
Preferably, above-mentioned step (5) is high-pressure homogeneous: by peanut shell fiber enzymolysis liquid obtained by step (4) first 200W's
Ultrasonic disperse 5-10min under power, supersonic frequency 20kHz, then homogeneous 4 times under the pressure of 400-800bar；For the first time
The condition of homogeneous is 400-600bar, and the condition of second of homogeneous is 500-600bar, and the condition of third time homogeneous is 700-
The condition of 800bar, the 4th homogeneous are 700-800bar.
The beneficial effects of the present invention are:
(1) present invention is abundance, cheap using peanut shell as raw material, not only instead of high-cost cotton, Asia
The raw materials such as fiber crops, and it is effectively utilized the by-product of peanut processing, it can produce huge economic benefit and social benefit.
(2) nano-cellulose prepared by the present invention utilizes steam explosion technology and high-pressure homogeneous method, and this method uses
Chemical reagent is few, short processing time, the remarkable advantage with high efficiency, low cost.
(3) nano-cellulose diameter prepared by the present invention is 5-25nm, length 70-190nm, has excellent mechanicalness
Energy and biocompatibility, crystallinity is high, draw ratio is big, large specific surface area, can be widely applied to medicine, food and functional material
Equal fields.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture (200nm) of the peanut shell nano-cellulose of embodiment 1 in the present invention；
Fig. 2 is the transmission electron microscope picture (100nm) of the peanut shell nano-cellulose of embodiment 1 in the present invention；
Fig. 3 is the diameter distribution profile of the peanut shell nano-cellulose of embodiment 1 in the present invention；
Fig. 4 is the staple diagram of the peanut shell nano-cellulose of embodiment 1 in the present invention；
Fig. 5 is the tensile strength figure of peanut shell nano-cellulose of the invention to starch base full degradable membrane；
Fig. 6 is the stretching die spirogram of peanut shell nano-cellulose of the invention to starch base full degradable membrane.
Specific embodiment
Next with reference to the accompanying drawings and detailed description the present invention will be further explained, so as to the technology of this field
Personnel know more about the present invention, but do not limit the present invention with this.
Embodiment 1
Steam blasting combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose, includes the following steps:
(1) it pre-processes: peanut husk as raw material being spent into ionized water cleaning, is dried, is crushed, sieve with 100 mesh sieve；
(2) steam blasting: add the water content of water regulating step (1) the peanut shell powder for 5wt%, swollen 12h, then
Material is placed in steam explosion chamber, steam blasting pressure is set as 3.0MPa, and the time is set as 20s, is washed after explosion treatment with 50 DEG C of hot water
And filter, filter residue is the peanut case fibre for removing most of hemicellulose, lignin；
(3) chlorite bleaching: gained filter residue in step (2) and deionized water are placed in instead by solid-liquid ratio 1:20 (g/mL)
It answers in kettle, is 4 using acetic acid adjustment pH value of solution, the NaClO of 15g/L is added2, the water bath with thermostatic control at 40 DEG C, stirring 3h, by filter residue
It is filtered after washing to neutrality, filter residue is the peanut case fibre for removing remaining hemicellulose, lignin；
(4) enzymolysis processing: the citrate-phosphate disodium hydrogen buffer solution for being 4.5 with pH is fine by peanut shell obtained by step (3)
Dimension is made into the aqueous dispersions of 2.5wt%, and cellulase is added, and enzyme dosage 2500U/g is placed in water bath with thermostatic control at 40 DEG C, stirs
6h, then 80 DEG C of water-bath 40min enzyme deactivations；
(5) high-pressure homogeneous: by the first ultrasonic disperse under the power of 200W of peanut shell fiber enzymolysis liquid obtained by step (4)
10min, supersonic frequency 20kHz, then homogeneous 4 times under the pressure of 400-800bar；
The condition of above 4 homogeneous is respectively: the condition of first time homogeneous is 400bar, and the condition of second of homogeneous is
600bar, the condition of third time homogeneous are 600bar, and the condition of the 4th homogeneous is 800bar.
(6) it is centrifuged, is freeze-dried: the high-pressure homogeneous solution of step (5) being centrifuged 15min through 10000r/min, in collection
Supernatant is freeze-dried up to peanut shell nano-cellulose powder by clear liquid.
Embodiment 2
Steam blasting combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose, includes the following steps:
(1) it pre-processes: peanut husk as raw material being spent into ionized water cleaning, is dried, is crushed, sieve with 100 mesh sieve；
(2) steam blasting: add the water content of water regulating step (1) the peanut shell powder for 20wt%, swollen 10h, so
Material is placed in steam explosion chamber afterwards, steam blasting pressure is set as 2.0MPa, and the time is set as 40s, with 60 DEG C of hot water wash after explosion treatment
It washs and filters, filter residue is the peanut case fibre for removing most of hemicellulose, lignin；
(3) chlorite bleaching: gained filter residue in step (2) and deionized water are placed in instead by solid-liquid ratio 1:20 (g/mL)
It answers in kettle, is 4.5 using acetic acid adjustment pH value of solution, the NaClO of 15g/L is added2, the water bath with thermostatic control at 50 DEG C, stir 5h, will filter
Wash heat is filtered after washing to neutrality, and filter residue is the peanut case fibre for removing remaining hemicellulose, lignin；
(4) enzymolysis processing: the citrate-phosphate disodium hydrogen buffer solution for being 4.5 with pH is fine by peanut shell obtained by step (3)
Dimension is made into the aqueous dispersions of 5wt%, and cellulase is added, and enzyme dosage 4000U/g is placed in water bath with thermostatic control at 45 DEG C, stirs
4.5h, then 80 DEG C of water-bath 40min enzyme deactivations；
(5) high-pressure homogeneous: by the first ultrasonic disperse under the power of 200W of peanut shell fiber enzymolysis liquid obtained by step (4)
10min, supersonic frequency 20kHz, then homogeneous 6 times under the pressure of 600bar；
(6) it is centrifuged, is freeze-dried: the high-pressure homogeneous solution of step (5) being centrifuged 15min through 10000r/min, in collection
Supernatant is freeze-dried up to peanut shell nano-cellulose powder by clear liquid.
Embodiment 3
Steam blasting combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose, includes the following steps:
(1) it pre-processes: peanut husk as raw material being spent into ionized water cleaning, is dried, is crushed, sieve with 100 mesh sieve；
(2) steam blasting: add the water content of water regulating step (1) the peanut shell powder for 30wt%, swollen 8h, then
Material is placed in steam explosion chamber, steam blasting pressure is set as 1.0MPa, and the time is set as 80s, is washed after explosion treatment with 60 DEG C of hot water
And filter, filter residue is the peanut case fibre for removing most of hemicellulose, lignin；
(3) chlorite bleaching: gained filter residue in step (2) and deionized water are placed in instead by solid-liquid ratio 1:20 (g/mL)
It answers in kettle, is 5 using acetic acid adjustment pH value of solution, the NaClO of 15g/L is added2, the water bath with thermostatic control at 60 DEG C, stirring 6h, by filter residue
It is filtered after washing to neutrality, filter residue is the peanut case fibre for removing remaining hemicellulose, lignin；
(4) enzymolysis processing: the citrate-phosphate disodium hydrogen buffer solution for being 5 with pH is by peanut case fibre obtained by step (3)
The aqueous dispersions of 10wt% are made into, cellulase is added, enzyme dosage 4500U/g is placed in water bath with thermostatic control at 45 DEG C, 6h is stirred,
Then 80 DEG C of water-bath 40min enzyme deactivations；
(5) high-pressure homogeneous: by the first ultrasonic disperse under the power of 200W of peanut shell fiber enzymolysis liquid obtained by step (4)
5min, supersonic frequency 20kHz, then homogeneous 3 times under the pressure of 800bar；
(6) it is centrifuged, is freeze-dried: the high-pressure homogeneous solution of step (5) being centrifuged 10min through 10000r/min, in collection
Supernatant is freeze-dried up to peanut shell nano-cellulose powder by clear liquid.
Embodiment 4
Steam blasting combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose, includes the following steps:
(1) it pre-processes: peanut husk as raw material being spent into ionized water cleaning, is dried, is crushed, sieve with 100 mesh sieve；
(2) steam blasting: add the water content of water regulating step (1) the peanut shell powder for 40wt%, swollen 6h, then
Material is placed in steam explosion chamber, steam blasting pressure is set as 0.5MPa, and the time is set as 100s, is washed after explosion treatment with 70 DEG C of hot water
And filter, filter residue is the peanut case fibre for removing most of hemicellulose, lignin；
(3) chlorite bleaching: gained filter residue in step (2) and deionized water are placed in instead by solid-liquid ratio 1:20 (g/mL)
It answers in kettle, is 5 using acetic acid adjustment pH value of solution, the NaClO of 15g/L is added2, the water bath with thermostatic control at 60 DEG C, stirring 6h, by filter residue
It is filtered after washing to neutrality, filter residue is the peanut case fibre for removing remaining hemicellulose, lignin；
(4) enzymolysis processing: the citrate-phosphate disodium hydrogen buffer solution for being 6 with pH is by peanut case fibre obtained by step (3)
The aqueous dispersions of 10wt% are made into, cellulase is added, enzyme dosage 5000U/g is placed in water bath with thermostatic control at 40 DEG C, stirs
4.5h, then 80 DEG C of water-bath 40min enzyme deactivations；
(5) high-pressure homogeneous: by the first ultrasonic disperse under the power of 200W of peanut shell fiber enzymolysis liquid obtained by step (4)
5min, supersonic frequency 20kHz, then homogeneous 4 times under the pressure of 800bar；
(6) it is centrifuged, is freeze-dried: the high-pressure homogeneous solution of step (5) being centrifuged 15min through 10000r/min, in collection
Supernatant is freeze-dried up to peanut shell nano-cellulose powder by clear liquid.
About the present invention, inventor has done some comparative experimentss, and the condition of experiment is specific as follows:
Comparative example 1
It is with the difference of embodiment 1, homogenization pressure is set as 200bar；Remaining condition is identical with embodiment 1；
Comparative example 2
It is with the difference of embodiment 1, homogenization cycles are set as 6 times, this 6 times processing condition is respectively: for the first time
The condition of homogeneous is 400bar, and the condition of second of homogeneous is 500bar, and the condition of third time homogeneous is 500bar, and the 4th time
The condition of matter is 600bar, and the condition of the 5th homogeneous is 600bar, and the condition of the 6th homogeneous is 800bar；Remaining condition with
Embodiment 1 is identical；
Comparative example 3
It is with the difference of embodiment 1, homogenization cycles are set as 2 times, this 2 times processing condition is respectively: for the first time
The condition of homogeneous is 600bar, and the condition of second of homogeneous is 800bar；Remaining condition is identical with embodiment 1；
Comparative example 4
It is with the difference of embodiment 1, step (6) centrifugation will be directly entered after step (4) enzymolysis processing, freezing is done
It is dry, during which without high-pressure homogeneous processing；Remaining step is identical with embodiment 1；
The product comparison sheet that the product of the invention of table 1 and sour water solution obtain
| Sample | Total production time (h) | Chemical reagent | Cost (member/500g) |
| Sour water solution | 57 | Acid | 21629 |
| Embodiment 1 | 29 | / | 11046 |
As it can be seen from table 1 the present invention is compared with acid-hydrolyzed method, time-consuming is short, at low cost.
The properties of product and cost comparison sheet that the product of the invention of table 2 and sour water solution obtain
By the data in above table, comparing embodiment 1 and comparative example 1 are as can be seen that the pressure of homogeneous is adjusted to
200bar, crystallinity, yield and the cost of obtained product reduce；Comparing embodiment 1 and comparative example 2 are as can be seen that will be equal
The number of matter rises to 6 times, and crystallinity, yield and the cost of obtained product improve；Comparing embodiment 1 and comparative example 3 can
To find out, the number of homogeneous is adjusted to 2 times, crystallinity, yield and the cost of obtained product reduce；Comparing embodiment 1
With comparative example 4 as can be seen that the yield and cost of obtained product are substantially reduced without high-pressure homogeneous.
Influence of the peanut shell nano-cellulose of the invention of table 3 to tapioca gelatinization characteristic
Table 3 is that peanut shell nano-cellulose prepared by the present invention (account for starch quality 5%) is gelatinized characteristic to tapioca
Influence, as shown in Table 3, the addition of peanut shell nano-cellulose, can be improved the peak paste viscosity of tapioca, valley viscosity,
Disintegration value, terminal viscosity, recycled LDPE and gelatinization point etc..
Fig. 5-6 is peanut shell nano-cellulose prepared by the present invention (account for starch quality 3%) to starch base full degradable membrane
The influence of mechanical performance, by Fig. 5-6 it is found that membrane material can be significantly improved by adding the peanut shell nano-cellulose of different embodiments
The tensile strength and stretch modulus of material illustrate that peanut shell nano-cellulose has relatively good reinforcing effect.
Comparative example 5
The present inventor also invented that a kind of effect is suitable with the present invention but the method for slightly different from, and specific steps are such as
Under:
(1) it pre-processes: peanut husk as raw material being spent into ionized water cleaning, is dried, is crushed, sieve with 100 mesh sieve, obtain peanut shell powder
End；
(2) steam blasting: add the water content of water regulating step (1) the peanut shell powder for 45wt%, swollen 16h, so
Material is placed in steam explosion chamber afterwards, sets steam blasting pressure as 0.5MPa, time 100s, with 70 DEG C of hot water wash after explosion treatment
It washs and filters, a resulting filter residue is the peanut case fibre for removing most of hemicellulose, lignin；
(3) chlorite bleaching: the resulting filter residue of step (2) is set with deionized water by solid-liquid ratio 1:20 (g/mL)
In reaction kettle, it is 4 using acetic acid adjustment pH value of solution, the NaClO of 15g/L is added2, the water bath with thermostatic control at 40 DEG C, stirring 4h, mistake
Filter, will filter after resulting secondary residue washing to neutrality, and secondary filter residue is the peanut shell for removing remaining hemicellulose, lignin
Fiber；
(4) enzymolysis processing: the disodium hydrogen phosphate-citric acid solution for being 4 with pH matches secondary filter residue obtained by step (3)
At the aqueous dispersions of 2wt%, cellulase is added, enzyme dosage 2000U/g is placed in water bath with thermostatic control at 45 DEG C, stirs 5h, then
Boiling water bath 20min enzyme deactivation；
(5) it is ultrasonically treated: peanut shell fiber enzymolysis liquid obtained by step (4) being ultrasonically treated 30min in ice-water bath, ultrasound
Power is 1500W, supersonic frequency 20kHz；
(6) it is centrifuged, is freeze-dried: the solution of step (5) ultrasonic treatment being centrifuged 5min through 10000r/min, collects supernatant
Supernatant is freeze-dried up to peanut shell nano-cellulose powder by liquid.
| Sample | Total production time (h) | Cost (member/500g) | Chemical reagent |
| Embodiment 1 | 29 | 11046 | / |
| Comparative example 5 | 29.5 | 11564 | / |
The method of comparative example 5 is also more prominent in save the cost and in terms of shortening the production time, but compares with the present invention,
The production time of comparative example 5 slightly long half an hour, the cost of product per jin will have more 8 yuans.As it can be seen that the present invention is relative to comparative example
5 be a kind of small improvement and progress again.
Above embodiments are one kind of the present invention more preferably specific embodiment, and those skilled in the art are in the technical program
The usual variations and alternatives carried out in range should be included within the scope of the present invention.
Claims (9)
1. a kind of steam blasting combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose, include the following steps:
(1) pre-process: cleaning peanut husk as raw material is dried, is crushed, and sieving obtains peanut shell powder；
(2) steam blasting: being added water in the peanut shell powder in (1), and after swollen 6-12h then steam blasting is washed with hot water
And filter, obtain a filter residue；
(3) chlorite bleaching: a filter residue in (2) is placed in reaction kettle, adjusts pH4-5, and NaClO is added2, thermostatted water
Bath, stirring filter after washing to neutrality, obtain secondary filter residue；
(4) enzymolysis processing: being made into aqueous dispersions for peanut case fibre obtained by (3), and cellulase, enzymatic hydrolysis, enzyme deactivation is added；
(5) high-pressure homogeneous: by peanut shell fiber enzymolysis liquid ultrasonic disperse obtained by (4), then homogeneous；
(6) it is centrifuged, is freeze-dried: the solution of (5) mesohigh homogeneous is centrifuged, collect supernatant, supernatant is freeze-dried, is obtained
Obtain peanut shell nano-cellulose powder.
2. a kind of steam blasting as described in claim 1 combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose,
It is characterized in that:
(1) it pre-processes: peanut husk as raw material being spent into ionized water cleaning, is dried, is crushed, sieve with 100 mesh sieve.
3. a kind of steam blasting as described in claim 1 combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose,
It is characterized in that:
(2) steam blasting: being added water in the peanut shell powder in (1), makes water content 5-40wt%, swollen 6-12h postposition
In steam explosion chamber, steam blasting pressure is set as 0.5-3.0MPa, explosion 20-100s, is washed simultaneously after explosion treatment with 50-70 DEG C of hot water
Filtering, obtains a filter residue.
4. a kind of steam blasting as described in claim 1 combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose,
It is characterized in that:
(3) filter residue of gained and deionized water in step (2) chlorite bleaching: are pressed into feed liquid mass volume ratio 1g:20mL
It is placed in reaction kettle, is 4-5 using acetic acid adjustment pH value of solution, the NaClO of 15g/L is added2, the water bath with thermostatic control at 40-60 DEG C stirs
3-6h is mixed, will be filtered after residue washing to neutrality, obtain secondary filter residue.
5. a kind of steam blasting as described in claim 1 combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose,
It is characterized in that:
(4) enzymolysis processing: secondary filter residue obtained by step (3) is prepared with the citrate-phosphate disodium hydrogen buffer solution that pH is 4-6
At the aqueous dispersions of 0.5-10wt%, cellulase is added, the dosage of cellulase is 400-5000U/g, is placed at 40-50 DEG C
4-6h, then 80 DEG C of water-bath 30-40min enzyme deactivations are stirred in water bath with thermostatic control.
6. a kind of steam blasting as described in claim 1 combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose,
It is characterized in that:
(5) high-pressure homogeneous: by the first ultrasonic disperse 5-10min under the power of 200W of peanut shell fiber enzymolysis liquid obtained by step (4),
Supersonic frequency is 20kHz, then homogeneous 3-6 times under the pressure of 400-800bar.
7. a kind of steam blasting as described in claim 1 combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose,
It is characterized in that:
(6) it is centrifuged, is freeze-dried: the high-pressure homogeneous solution of step (5) being centrifuged 5-15min through 10000r/min, collects supernatant
Supernatant is freeze-dried up to peanut shell nano-cellulose powder by liquid.
8. a kind of steam blasting as described in claim 1 combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose, packet
Include following step:
(1) it pre-processes: peanut husk as raw material being spent into ionized water cleaning, is dried, is crushed, sieve with 100 mesh sieve
(2) steam blasting: being added water in the peanut shell powder in (1), makes water content 5-40wt%, swollen 6-12h postposition
In steam explosion chamber, steam blasting pressure is set as 0.5-3.0MPa, explosion 20-100s, is washed simultaneously after explosion treatment with 50-70 DEG C of hot water
Filtering, obtains a filter residue；
(3) chlorite bleaching: filter residue of gained in (2) and deionized water are placed in by feed liquid mass volume ratio 1g:20mL
In reaction kettle, it is 4-5 using acetic acid adjustment pH value of solution, the NaClO of 15g/L is added2, the water bath with thermostatic control at 40-60 DEG C, stirring 3-
6h will filter after residue washing to neutrality, obtain secondary filter residue；
(4) enzymolysis processing: secondary filter residue obtained by step (3) is prepared with the citrate-phosphate disodium hydrogen buffer solution that pH is 4-6
At the aqueous dispersions of 0.5-10wt%, cellulase is added, the dosage of cellulase is 400-5000U/g, is placed at 40-50 DEG C
4-6h, then 80 DEG C of water-bath 30-40min enzyme deactivations are stirred in water bath with thermostatic control；
(5) high-pressure homogeneous: by the first ultrasonic disperse 5-10min under the power of 200W of peanut shell fiber enzymolysis liquid obtained by step (4),
Supersonic frequency is 20kHz, then homogeneous 3-6 times under the pressure of 400-800bar；
(6) it is centrifuged, is freeze-dried: the high-pressure homogeneous solution of step (5) being centrifuged 5-15min through 10000r/min, collects supernatant
Supernatant is freeze-dried up to peanut shell nano-cellulose powder by liquid.
9. a kind of steam blasting as described in claim 1 combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose,
It is characterized in that:
(5) high-pressure homogeneous: by the first ultrasonic disperse 5-10min under the power of 200W of peanut shell fiber enzymolysis liquid obtained by step (4),
Supersonic frequency is 20kHz, then homogeneous 4 times under the pressure of 400-800bar；The condition of first time homogeneous is 400-600bar,
The condition of second of homogeneous is 500-600bar, and the condition of third time homogeneous is 700-800bar, and the condition of the 4th homogeneous is
700-800bar。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811191962.4A CN109338781A (en) | 2018-10-12 | 2018-10-12 | A kind of steam blasting combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose |
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| CN109750547A (en) * | 2019-03-07 | 2019-05-14 | 德宏州制糖工业研究所 | A method of nano-cellulose is prepared using sugaring by-product bagasse |
| CN109972437A (en) * | 2019-04-28 | 2019-07-05 | 吉林大学 | A method of nano-cellulose is prepared using apple pomace |
| CN110078959A (en) * | 2019-05-08 | 2019-08-02 | 台州学院 | A kind of wild rice stem waste liquified cellulosic film and preparation method thereof |
| CN110396140A (en) * | 2019-08-19 | 2019-11-01 | 华南理工大学 | A kind of method and its application of pectin decoloration |
| CN112674320A (en) * | 2021-02-02 | 2021-04-20 | 山东东兴源食品有限公司 | Fermented ginger seasoning noodle sauce powder and preparation method thereof |
| CN113073485A (en) * | 2021-04-09 | 2021-07-06 | 黑龙江八一农垦大学 | Preparation method of nano cellulose fiber and product thereof |
| CN114197233A (en) * | 2021-12-17 | 2022-03-18 | 大连理工大学 | Method for separating and extracting cellulose nanofibers from agricultural and forestry solid wastes |
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| CN114197233B (en) * | 2021-12-17 | 2022-12-02 | 大连理工大学 | Method for separating and extracting cellulose nanofibers from agricultural and forestry solid wastes |
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