CN106087505A - A kind of preparation method of biomass cellulose nanofibers - Google Patents
A kind of preparation method of biomass cellulose nanofibers Download PDFInfo
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- CN106087505A CN106087505A CN201610443433.3A CN201610443433A CN106087505A CN 106087505 A CN106087505 A CN 106087505A CN 201610443433 A CN201610443433 A CN 201610443433A CN 106087505 A CN106087505 A CN 106087505A
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- sodium chlorite
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- fiber
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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
- D21C3/00—Pulping cellulose-containing materials
- D21C3/04—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides
-
- 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
- D21C3/00—Pulping cellulose-containing materials
- D21C3/18—Pulping cellulose-containing materials with halogens or halogen-generating compounds
-
- 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
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/001—Modification of pulp properties
- D21C9/007—Modification of pulp properties by mechanical or physical means
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Paper (AREA)
Abstract
The invention discloses the preparation method of a kind of biomass cellulose nanofibers.Including weighing biomass fiber and benzene alcoholic solution for 1:50～100 in mass ratio, it is then added to sodium chlorite solution, mixes with KOH solution, heat in being sealed by water-bath；Then ultrasonic Treatment and sided corona treatment are carried out；Nanofiber suspension carries out lyophilization, supercritical drying or critical point drying.Biomass fiber is extracted by the present invention through benzene alcoholic solution, removes the solable matter in biomass fiber, then removes lignin, KOH solution removing hemicellulose, removing lignin and hemicellulose the most again with sodium chlorite；With the HCl treatment removing insoluble hemicellulose of alkali and lignin, last ultrasonic disruption processes, then carries out corona and hit stream and obtain having high length-diameter ratio, high biomass cellulose nanofibers, has the distribution of more preferable fiber, microhomogeneity can be good, has more preferable mechanical property.
Description
Technical field
The invention belongs to biomass technical field, particularly relate to the preparation side of a kind of biomass cellulose nanofibers
Method.
Background technology
The physical property of nano material is different from conventional material.Such as, the fusing point of nanometer gold is far below the fusing point of normality gold
(1064 DEG C), and particle size is the least, and fusing point is the lowest: when particle radius is 5nm, 3nm and 2nm, fusing point is respectively 900
DEG C, 770 DEG C and 500 DEG C.The color of nano material also tends to be different from conventional material.Such as, gold is yellow, and nanometer gold is then
Take on a red color.Nanotechnology can also change the surface property of material.Such as, the glass processed through the nano TiO 2 broken through with water
Glass is it can be clearly seen that material object below, but does not sees thing below on untreated glass surface because of the striped of water
Body.
Timber/lignocellulose be a kind of generally exist contain the abundantest natural biology resource, there is nanoscale
Fibre structure, and there is controlled " self assembly " (Self-assembly) performance.As a kind of nano material, timber/wooden fibre
Dimension element is also far from obtaining sufficient development and utilization with the interaction of other nano materials, also can develop a variety of function
With purposes, meanwhile, the new technique being applied to biological material analysis is applied in lignocellulose field, can develop wooden fibre
More new application of dimension element, therefore, the research of lignocellulose will become the basis of exploitation biomass resource sustainability economy.
Owing to cellulosic molecule interchain exists higher Hyarogen-bonding so that mutually the most interpolymerized between the nanofiber of preparation
The integrated diameter fiber aggregate higher than 100nm, this few fibers is difficult to dispersed in use, have impact on reinforced effects；
Utilize fermentable to prepare Bacterial cellulose, can prepare that diameter size distribution is uniform, the high length-diameter ratio nanometer of netted entanglement
Fiber, but the preparation cost of this material is higher, and the requirement to preparation condition and preparation process is the harshest, have impact on and receives
The production efficiency of rice fiber and economic benefit.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of biomass cellulose nanofibers, by biomass are fine
Tie up and extract through benzene alcoholic solution, remove the solable matter in biomass fiber, then remove lignin, KOH solution with sodium chlorite
Removing hemicellulose, the most again removing lignin and hemicellulose；With the HCl treatment removing insoluble hemicellulose of alkali and wooden
Element, last ultrasonic disruption processes, then carries out corona, obtains a kind of high-quality biological matter cellulose nano-fibrous.
For solving above-mentioned technical problem, the present invention is achieved by the following technical solutions:
The present invention is the preparation method of a kind of biomass cellulose nanofibers, comprises the steps,
Step one: weigh biomass fiber and benzene alcoholic solution for 1:50～100 in mass ratio, and biomass fiber is placed in
In benzene alcoholic solution, under conditions of temperature is 85 DEG C～95 DEG C, extract 5h～7h；
Step 2: preparation mass concentration is the sodium chlorite solution of 1%～2%, and to regulate its pH value be 4～5, then will
The biomass fiber processed through step one joins holding 4h～6h in sodium chlorite solution, and period continues every 0.9～1.1h
Sodium chlorite and glacial acetic acid is added, to keep the mass concentration of sodium chlorite in sodium chlorite solution to be in sodium chlorite solution
1%～2%, the pH value of sodium chlorite solution is 4～5；
Step 3: the biomass fiber processed through step 2 is joined the KOH that mass concentration is 1.5%～2.5% molten
In liquid, mix homogeneously, under the conditions of temperature is 80 DEG C～100 DEG C, keep 1.5h～2.5h；
Step 4: add 0.4mL～0.6mL glacial acetic acid and 0.5g～0.7g sodium chlorite by 63mL～67mL distilled water
Ratio, joins glacial acetic acid and sodium chlorite and makes solution in distilled water, and added by the biomass fiber processed through step 3
Enter in solution, seal heat treated 0.8h～1.2h in the water-bath being placed on 72 DEG C～77 DEG C；
Step 5: the biomass fiber after step 4 processes is joined the KOH that mass concentration is 4.5%～5.5%
In solution, mix homogeneously, under the conditions of temperature is 80 DEG C～100 DEG C, keep 1.5h～2.5h；
Step 6: the biomass fiber after step 5 processes is joined the hydrochloric acid that mass concentration is 0.8%～1.2%
In, seal and the water-bath being placed on 75 DEG C～85 DEG C heats 1.8h～2.2h；
Step 7: be added to the water by the biomass fiber after step 6 processes, then carries out ultrasonic Treatment, ultrasonic
Power is 400W～2000W, and ultrasonic time is 5min～30min, obtains nanofiber suspension；
Step 8: nanofiber suspension step 7 obtained carries out sided corona treatment, the corona time is 30s-60s；
Step 9: the nanofiber suspension obtained through step 8 is carried out lyophilization, supercritical drying or critical
Point is dried.
Further, the biomass fiber described in described step one is 50 mesh～the wood fiber of 70 mesh, 50 mesh～70 mesh
Bamboo fibre, 50 mesh～the cotton fiber of 70 mesh, 50 mesh～the flaxen fiber of 70 mesh.
Further, described step 2 is prepared the sodium chlorite solution that mass concentration is 1.1%～1.9%, and regulates
Its pH value is 4.2～4.8, then the biomass fiber processed through step one is joined in sodium chlorite solution keep 4.2h～
5.8h, period adds sodium chlorite and glacial acetic acid every 0.95～1.05h in sodium chlorite solution, to keep sodium chlorite molten
In liquid, the mass concentration of sodium chlorite is 1.1%～1.9%, and the pH value of sodium chlorite solution is 4.2～4.8.
Further, described step 4 is pressed 64mL～66mL distilled water add 0.44mL～0.55mL glacial acetic acid and
The ratio of 0.55g～0.65g sodium chlorite, joins glacial acetic acid and sodium chlorite and makes solution in distilled water.
Further, the biomass fiber processed through step 3 is joined in solution by described step 4, seal rearmounted
Heat treated 0.9h～1.1h in the water-bath of 73 DEG C～76 DEG C.
The method have the advantages that
Biomass fiber is extracted by the present invention through benzene alcoholic solution, removes the solable matter in biomass fiber, then with sub-
Sodium chlorate removing lignin, KOH solution removing hemicellulose, removing lignin and hemicellulose the most again；Use HCl treatment
The removing insoluble hemicellulose of alkali and lignin, last ultrasonic disruption processes, then carry out corona hit stream obtain having high length-diameter ratio,
High biomass cellulose nanofibers, has the distribution of more preferable fiber, and microhomogeneity can be good, has more preferable mechanics
Performance.
Certainly, the arbitrary product implementing the present invention it is not absolutely required to reach all the above advantage simultaneously.
Detailed description of the invention
Technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is only
The a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art
The all other embodiments obtained under not making creative work premise, broadly fall into the scope of protection of the invention.
The present invention is the preparation method of a kind of biomass cellulose nanofibers, comprises the steps,
Step one: weigh biomass fiber and benzene alcoholic solution for 1:50～100 in mass ratio, and biomass fiber is placed in
In benzene alcoholic solution, under conditions of temperature is 85 DEG C～95 DEG C, extract 5h～7h；
Step 2: preparation mass concentration is the sodium chlorite solution of 1%～2%, and to regulate its pH value be 4～5, then will
The biomass fiber processed through step one joins holding 4h～6h in sodium chlorite solution, and period continues every 0.9～1.1h
Sodium chlorite and glacial acetic acid is added, to keep the mass concentration of sodium chlorite in sodium chlorite solution to be in sodium chlorite solution
1%～2%, the pH value of sodium chlorite solution is 4～5；
Step 3: the biomass fiber processed through step 2 is joined the KOH that mass concentration is 1.5%～2.5% molten
In liquid, mix homogeneously, under the conditions of temperature is 80 DEG C～100 DEG C, keep 1.5h～2.5h；
Step 4: add 0.4mL～0.6mL glacial acetic acid and 0.5g～0.7g sodium chlorite by 63mL～67mL distilled water
Ratio, joins glacial acetic acid and sodium chlorite and makes solution in distilled water, and added by the biomass fiber processed through step 3
Enter in solution, seal heat treated 0.8h～1.2h in the water-bath being placed on 72 DEG C～77 DEG C；
Step 5: the biomass fiber after step 4 processes is joined the KOH that mass concentration is 4.5%～5.5%
In solution, mix homogeneously, under the conditions of temperature is 80 DEG C～100 DEG C, keep 1.5h～2.5h；
Step 6: the biomass fiber after step 5 processes is joined the hydrochloric acid that mass concentration is 0.8%～1.2%
In, seal and the water-bath being placed on 75 DEG C～85 DEG C heats 1.8h～2.2h；
Step 7: be added to the water by the biomass fiber after step 6 processes, then carries out ultrasonic Treatment, ultrasonic
Power is 400W～2000W, and ultrasonic time is 5min～30min, obtains nanofiber suspension；
Step 8: nanofiber suspension step 7 obtained carries out sided corona treatment, the corona time is 30s-60s；
Step 9: the nanofiber suspension obtained through step 8 is carried out lyophilization, supercritical drying or critical
Point is dried.
Wherein, the biomass fiber described in step one be 50 mesh～the wood fiber of 70 mesh, 50 mesh～the bamboo fibre of 70 mesh,
50 mesh～the cotton fiber of 70 mesh, 50 mesh～the flaxen fiber of 70 mesh.
Wherein, preparing mass concentration in step 2 is the sodium chlorite solution of 1.1%～1.9%, and regulates its pH value and be
4.2～4.8, then the biomass fiber processed through step one is joined holding 4.2h～5.8h, phase in sodium chlorite solution
Between in sodium chlorite solution, add sodium chlorite and glacial acetic acid every 0.95～1.05h, to keep the sodium chlorite solution Central Asia
The mass concentration of sodium chlorate is 1.1%～1.9%, and the pH value of sodium chlorite solution is 4.2～4.8.
Wherein, step 4 is pressed 64mL～66mL distilled water and adds 0.44mL～0.55mL glacial acetic acid and 0.55g～0.65g
The ratio of sodium chlorite, joins glacial acetic acid and sodium chlorite and makes solution in distilled water.
Wherein, the biomass fiber processed through step 3 is joined in solution by step 4, seal be placed on 73 DEG C～
Heat treated 0.9h～1.1h in the water-bath of 76 DEG C.
In the description of this specification, the description of reference term " embodiment ", " example ", " concrete example " etc. means
The specific features that describes in conjunction with this embodiment or example, structure, material are lived feature and are contained at least one of the present invention and implement
In example or example.In this manual, the schematic representation to above-mentioned term is not necessarily referring to identical embodiment or example.
And, the specific features of description, structure, material or feature can be to close in any one or more embodiments or example
Suitable mode combines.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.Preferred embodiment is the most detailed
Describe all of details, be also not intended to the detailed description of the invention that this invention is only described.Obviously, according to the content of this specification,
Can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is to preferably explain the present invention
Principle and actual application so that skilled artisan can be best understood by and utilize the present invention.The present invention is only
Limited by claims and four corner thereof and equivalent.
Claims (5)
1. the preparation method of a biomass cellulose nanofibers, it is characterised in that: comprise the steps,
Step one: weigh biomass fiber and benzene alcoholic solution for 1:50～100 in mass ratio, and biomass fiber is placed in benzene alcohol
In solution, under conditions of temperature is 85 DEG C～95 DEG C, extract 5h～7h；
Step 2: preparation mass concentration is the sodium chlorite solution of 1%～2%, and to regulate its pH value be 4～5, then will be through step
Rapid one biomass fiber processed joins holding 4h～6h in sodium chlorite solution, and period continues to Asia every 0.9～1.1h
Sodium chlorate solution adds sodium chlorite and glacial acetic acid, to keep in sodium chlorite solution the mass concentration of sodium chlorite for 1%
～2%, the pH value of sodium chlorite solution is 4～5；
Step 3: the biomass fiber processed through step 2 is joined in the KOH solution that mass concentration is 1.5%～2.5%,
Mix homogeneously, keeps 1.5h～2.5h under the conditions of temperature is 80 DEG C～100 DEG C；
Step 4: add 0.4mL～0.6mL glacial acetic acid and the ratio of 0.5g～0.7g sodium chlorite by 63mL～67mL distilled water
Example, joins glacial acetic acid and sodium chlorite and makes solution in distilled water, and is added by the biomass fiber processed through step 3
In solution, seal heat treated 0.8h～1.2h in the water-bath being placed on 72 DEG C～77 DEG C；
Step 5: the biomass fiber after step 4 processes is joined the KOH solution that mass concentration is 4.5%～5.5%
In, mix homogeneously, under the conditions of temperature is 80 DEG C～100 DEG C, keep 1.5h～2.5h；
Step 6: the biomass fiber after step 5 processes is joined in the hydrochloric acid that mass concentration is 0.8%～1.2%,
Seal to be placed in the water-bath of 75 DEG C～85 DEG C and heat 1.8h～2.2h；
Step 7: be added to the water by the biomass fiber after step 6 processes, then carries out ultrasonic Treatment, ultrasonic power
For 400W～2000W, ultrasonic time is 5min～30min, obtains nanofiber suspension；
Step 8: nanofiber suspension step 7 obtained carries out sided corona treatment, the corona time is 30s-60s；
Step 9: the nanofiber suspension obtained through step 8 is carried out lyophilization, supercritical drying or critical point and does
Dry.
The preparation method of a kind of biomass cellulose nanofibers the most according to claim 1, it is characterised in that described step
Biomass fiber described in rapid one is 50 mesh～the wood fiber of 70 mesh, 50 mesh～the bamboo fibre of 70 mesh, 50 mesh～the cotton of 70 mesh
Fiber, 50 mesh～the flaxen fiber of 70 mesh.
The preparation method of a kind of biomass cellulose nanofibers the most according to claim 1, it is characterised in that described step
Preparing mass concentration in rapid two is the sodium chlorite solution of 1.1%～1.9%, and to regulate its pH value be 4.2～4.8, then will
The biomass fiber processed through step one joins in sodium chlorite solution holding 4.2h～5.8h, period every 0.95～
1.05h adds sodium chlorite and glacial acetic acid in sodium chlorite solution, to keep the quality of sodium chlorite in sodium chlorite solution
Concentration is 1.1%～1.9%, and the pH value of sodium chlorite solution is 4.2～4.8.
The preparation method of a kind of biomass cellulose nanofibers the most according to claim 1, it is characterised in that described step
0.44mL～0.55mL glacial acetic acid and the ratio of 0.55g～0.65g sodium chlorite is added in 64mL～66mL distilled water in rapid four,
Glacial acetic acid and sodium chlorite are joined distilled water is made solution.
The preparation method of a kind of biomass cellulose nanofibers the most according to claim 1, it is characterised in that described step
In rapid four, the biomass fiber processed through step 3 is joined in solution, seal in the water-bath being placed on 73 DEG C～76 DEG C and add
Heat treatment 0.9h～1.1h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108164717A (en) * | 2017-12-28 | 2018-06-15 | 北京林业大学 | A kind of method that 3D printing cellulose reinforcing material is extracted from timber |
| CN110080025A (en) * | 2019-05-06 | 2019-08-02 | 南京林业大学 | Regulate and control the method and its application of cellulose size |
| CN116676799A (en) * | 2023-06-29 | 2023-09-01 | 广东食品药品职业学院 | Preparation method and application of apocynum cellulose |
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Address after: Granite County of Hefei City, Anhui province 231243 Feixi Zhenyuan Sun Ji Xiang textile factory Applicant after: Anhui new agricultural Limited by Share Ltd Address before: Granite County of Hefei City, Anhui province 231243 Feixi Zhenyuan Sun Ji Xiang textile factory Applicant before: ANHUI XINSHENGLI BIOLOGY TECHNOLOGY CO., LTD. |
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Application publication date: 20161109 |