CN102174612A - Biological and mechanical silk dividing method for producing nanocellulose - Google Patents
Biological and mechanical silk dividing method for producing nanocellulose Download PDFInfo
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- CN102174612A CN102174612A CN2011100021080A CN201110002108A CN102174612A CN 102174612 A CN102174612 A CN 102174612A CN 2011100021080 A CN2011100021080 A CN 2011100021080A CN 201110002108 A CN201110002108 A CN 201110002108A CN 102174612 A CN102174612 A CN 102174612A
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Abstract
The invention provides a biological and mechanical silk dividing method for producing nanocellulose, which comprises the following steps of: firstly, the preparation of sugar-containing paper pulp: selecting refined paper pulp to immerse in a sugar solution, uniformly mixing the solution, and drying the paper pulp after the paper pulp is swelled up for 24h to form the sugar-containing paper pulp; secondly, the preparation of materials to be fermented: uniformly mixing bran, peptone and yeast with the sugar-containing paper pulp at a certain weight ratio, and regulating the pH value to be 6; thirdly, filling the mixture in a container for fermentation, controlling the temperature between 30 DEG C and 35 DEG C, and fermenting the mixture for 70-75h, wherein fermented pulp material is produced when the scent of wine can be smelt; and fourthly, the grinding of fermentation pulp: after water is added into the fermentation pulp, putting the fermentation pulp into a grinding machine to repeatedly grind 5-15 times to form a colloidal solution of the nanocellulose, and filtering the solution or lyophilizing the solution in vacuum to obtain the product. The method for producing the nanocellulose has little influence on fiber strength, has no damage on the container, and has no pollution on the environment; moreover, the prepared nanocellulose is branch-shaped, and therefore, the prepared composite material has good compositionality, mechanical properties and thermal performance.
Description
Technical field
The present invention relates to a kind of manufacture method of nanofiber rope.It is to be raw material with the refined pulp, and the branch silk method that combines through microbial fermentation and mechanical mill makes nano-cellulose.
Background technology
The basic substance of vegetable fibre is a Mierocrystalline cellulose, and it is a natural polymer the abundantest on the earth, the most valuable human natural reproducible resource.It is different purposes properties of materials with sex change that fiber have processing, therefore, utilizes cellulosic this specific character in recent years, produces various matrix materials, is widely used in each field of national economy.
As everyone knows, deficiencies such as cellulosic not resistance to chemical attack, intensity difference and physical aspect have limited its range of application to a certain extent.Compare with the conventional fibre element through the nanoscale Mierocrystalline cellulose that the nanometer decentralized system gets, because of characteristics such as its high purity, high-crystallinity, high elastic coefficient, high strength, with it is that the matrix material of wild phase has shown high Young's modulus, intensity, thermostability, rigidity and snappiness etc., its lightweight, degradable, physiologically acceptable and characteristic such as renewable make it demonstrate great application prospect in high performance composite in addition.The nano-cellulose surface comprises a large amount of hydroxyls, makes its surface be easy to chemical modification, thereby gives the surface different characteristics.Can make the hydrophobic base material have dispersiveness by surface modification, enlarge the range of application of nano-cellulose.In addition, nano-cellulose also has the potential application prospect in fields such as optical material, black plate agent material and intelligent materials.
Plant cellulose fibrous texture complexity, the degree of crystallinity height, the nanometer difficulty is higher.Domestic and international most of nano-cellulose preparation method is based on chemical method, as hydrolysis method, solvent method, ion liquid dissolving method etc. at present.These methods are all with first dissolving cellulos, and back recrystallize generates and the original different new crystal modification of cell configuration, i.e. nano whisker.But this nano whisker has destroyed the linear giant molecule structure that original glycosidic link is formed by connecting, and the polymerization degree reduces, the mechanical property variation, and the production process environmental pollution is big, and equipment corrosion is serious, and the suitability for industrialized production ability is also lower.
Also there is physical methods such as adopting ultrasonic grinding to make nano-cellulose, as:
US2010/0065236 discloses a kind of patented technology of using the high-pressure homogeneous manufactured nano-cellulose of physics, CN101691698 discloses and has a kind ofly carried out chemical treatment with phenylethyl alcohol and Glacial acetic acid, make the patented technology of nano-cellulose again in conjunction with the ultrasonic disruption facture, these technology, the manufacturing that is nano-cellulose provides a kind of new approach, and the society of respectively doing for oneself makes contributions.But say on the whole, physical treatment process such as high-pressure homogeneous or ultrasonic wave, fiber surface easily produces hole, influences intensity, and container is damaged to some extent.By retrieval, do not find as yet to divide silk method to make the document announcement of nano-cellulose with biological fermentation and mechanical mill bonded.
Summary of the invention
The technical problem to be solved in the present invention is to design a kind of biological fermentation of nano-cellulose and branch silk method that mechanical mill combines made.
The technical scheme that solves this technical problem employing is: the bio-mechanical of this manufacturing nano-cellulose divides silk method process the following step:
(1) preparation contains the candy paper slurry: with water ratio is the refined pulp of 10%-15%, and being immersed in process water is that 95 weight parts and sucrose are in the sugar aqueous solution of 5 weight parts, fully stirs, and behind the swollen 24h, pulls the candy paper that contains that drains into water ratio 60%-70% out and starches;
(2) treat the preparation of fermented product: be mixed with following raw materials according and weight part thereof, the water ratio that 50 parts of wheat brans, 2.5 parts of peptones, 2 parts of yeast, 1000 parts of steps (1) make be 60%-70% contain the candy paper slurry, mix and fully mix thoroughly and become to treat fermented product, the pH value is 6;
(3) pack into container fermentation: the mixing that step (2) is made is mixed thoroughly treats to place Altar or plastics bag partly to seal by fermented product, and controlled temperature 30-35 ℃, fermentation 70-75h gives out slightly sour-sweet pungent wine flavour, then ferments successfully, becomes the fermentation slurry;
(4) grinding of fermentation slurry: with 1 weight part ferment slurry mix with 5 weight part process waters mix thoroughly after, put into nano-milled machine and grind 5-15 time repeatedly, nano-cellulose colloidal solution;
(5) filtration of colloidal solution or drying: press customer requirements or, nano-cellulose colloidal solution is carried out membrane filtration or vacuum lyophilization powdered for convenient storing.
Said yeast is the FWZ8-12 yeast powder.
Said nano-milled machine is the Japanese stone mortar formula masher that increases the two millstone types of MKCA6-3 of good fortune Co., Ltd. production and sales, and regulating abrasive disk space is 1-30 μ m.
The invention has the beneficial effects as follows: adopt present method little to the influence of fibre strength, do not damage container, production process is free from environmental pollution, make nano-cellulose and be dendroid through transmission electron microscope observing, such structure reflects that intuitively this nano-cellulose and other material are compound, and its composite performance, mechanical property and thermal characteristics are higher.
Description of drawings
Accompanying drawing is this nano-cellulose transmission electron microscope image.
Embodiment
The present invention is described in further detail below in conjunction with embodiment: the described refined pulp of step (1) comprises refining wood pulp, refining bamboo pulp, refining cotton pulp etc.The said sugar that contains in the candy paper slurry can be glucose, fructose, honey etc., from the consideration that is easy to get of low-cost and raw material, selects sucrose for use.Select for use refined pulp be raw material be because of its degree of crystallinity and the polymerization degree than common paper pulp height, the bonding force between cellulosic molecule and the molecule is big, carrying out nanometer, to divide a difficulty big relatively.Set about from difficulty, just select refined pulp for use, in case success, all the other easier processing.Certainly available various vegetable fibres are made final nano-cellulose as raw material, but this needs that vegetable fibre is done early stage and handles, as remove xylogen, hemicellulose etc., and these are routine techniques or prior art, nothing innovation part, therefore directly make raw material with refined pulp.Wheat bran, peptone, yeast in the step (2) all are commercially available, be conventional commodity, they are with sugar, and for paper pulp provides ferment required yeast and substratum thereof, wherein the yeast of 2 weight parts is to be the fixed value of example by commercially available FWZ8-12 yeast powder, other is as selecting commercially available distiller's yeast etc. for use, can be according to carrying out, the amount of adding also should remake correction, during actually operating, the yeast add-on is flexible slightly also substantially irrelevant, and available fermentation time length remedies.The Altar general reference container of dress Altar fermentation is not limited to the Altar jar in the step (3).Said partly seal finger with lid such as Sha Bu or air-permeable envelope or cover uncovered, in order to sneaking into of the assorted bacterium of insulation, oxygen supply and minimizing.Said nano-milled machine selects for use Japan to increase the stone mortar formula masher of the two mills of MKCA6-3 of good fortune Co., Ltd. in the step (4), adjusting abrasive disk space is 1-30 μ m, grind 5-15 time repeatedly, the Mierocrystalline cellulose that grinds often is thinner, but physical strength detracts thereupon to some extent.The filtration or the drying of step (5), the subsequent disposal operation after belonging to nano-cellulose and making.
Because of cellulose crystallity and polymerization degree height, refined pulp more so, be difficult for degraded, be to lay foundation through the syrup swollen earlier for preparing saccharomycetic substratum, also infiltrate noncrystalline domain to yeast and provide convenience, under the zymic fermentative action, fiber divides silk, Degradation by chemistry of micro-organisms power, reduced the degree of crystallinity and the polymerization degree, further ground again, under the compression that in grinding at a high speed, produces and the stress of shearing with nano-milled machine, be able to branch silk and degraded again, grind repeatedly, the degree of crystallinity of refined pulp and the polymerization degree are seriously lost, the fiber bundle-like body disintegrates, reach the purpose of branch silk, obtain nano-cellulose.
Embodiment 1: with the refined pulp of water ratio 10%, be immersed in the process water and the 5 weight part sucrose blended aqueous solution of 95 weight parts, fully stir, swollen 24h, pull out drain into water ratio be 60% contain the candy paper slurry; Aforementioned water ratio with 1000 weight parts is that 60% the wheat bran that contains candy paper slurry, 50 weight parts, the peptone and the mixing of 2 weight part FWZ8-12 yeast powders of 2.5 weight parts are mixed thoroughly again, makes and treats fermented product, and the pH value is 6; This is treated the fermented product Altar part omitted compacting of packing into, double-deck husky cloth on the Altar flap 30 ℃ temperature condition bottom fermentations 75 hours, is smelt wine flavour and is and ferments successfully, becomes the fermentation slurry again; Be 1: 5 mixed again with this fermentation slurry and process water with weight ratio, put into the stone mortar formula masher that Japan increases the two millstone types of MKCA6-3 of production of good fortune Co., Ltd. and sale, abrasive disk space 30 μ m, grind repeatedly 5 times, use membrane filtration, the mean diameter that gets fiber is about 100nm, length-to-diameter ratio is about 1500 nano-cellulose.
Embodiment 2: with water ratio is that 13% refined pulp is a raw material, make with embodiment 1 same procedure and to contain candy paper slurry, drain back water ratio 65%, refabrication is treated fermented product, leavening temperature is 32 ℃, fermentation 73h the fermentation slurry, the fermentation slurry is converted the stone mortar formula masher of putting into two millstone types behind the water, regulates abrasive disk space 15 μ m, grind repeatedly 10 times, vacuum lyophilization is powdered, and the mean diameter that gets fiber is about 60nm, and length-to-diameter ratio is about 1700 nano-cellulose.
Embodiment 3: the refined pulp with water ratio 15% is a raw material, make drain the back water ratio be 70%-contain candy paper slurry, refabrication is treated fermented product, send out temperature pure 35 ℃, fermentation 70h the fermentation slurry, put into masher after the fermentation slurry is converted water, spacing is transferred to 1 μ m and is ground repeatedly 15 times, vacuum-drying is powdered again behind membrane filtration, and the mean diameter that gets fiber is about 20nm, and length-to-diameter ratio is about 2000 nano-cellulose.
Unlisted parameter and concrete steps among the above embodiment 2,3, identical with embodiment 1, do not repeat.Be interval value only, make embodiment by lower value, intermediate value, higher limit apportion respectively parameter in each step.
Claims (3)
1. a bio-mechanical of making nano-cellulose divides silk method, it is characterized in that through the following step:
(1) preparation contains the candy paper slurry: with water ratio is the refined pulp of 10%-15%, and being immersed in process water is that 95 weight parts and sucrose are in the sugar aqueous solution of 5 weight parts, fully stirs, and behind the swollen 24h, pulls the candy paper that contains that drains into water ratio 60%-70% out and starches;
(2) treat the preparation of fermented product: be mixed with following raw materials according and weight part thereof, the water ratio that 50 parts of wheat brans, 2.5 parts of peptones, 2 parts of yeast, 1000 parts of steps (1) make be 60%-70% contain the candy paper slurry, mix and fully mix thoroughly and become to treat fermented product, the pH value is 6;
(3) pack into container fermentation: the mixing that step (2) is made is mixed thoroughly treats to place Altar or plastics bag partly to seal by fermented product, and controlled temperature 30-35 ℃, fermentation 70-75h gives out slightly sour-sweet pungent wine flavour, then ferments successfully, becomes the fermentation slurry;
(4) grinding of fermentation slurry: with 1 weight part ferment slurry mix with 5 weight part process waters mix thoroughly after, put into nano-milled machine and grind 5-15 time repeatedly, nano-cellulose colloidal solution;
(5) filtration of colloidal solution or drying: press customer requirements or, nano-cellulose colloidal solution is carried out membrane filtration or vacuum lyophilization powdered for convenient storing.
2. the bio-mechanical of manufacturing nanofiber as claimed in claim 1 divides silk method, it is characterized in that said yeast is the FWZ8-12 yeast powder.
3. the bio-mechanical of manufacturing nanofiber as claimed in claim 1 divides silk method, it is characterized in that said nano-milled machine is the Japanese stone mortar formula masher that increases the two millstone types of MKCA6-3 of good fortune Co., Ltd. production and sales, and regulating abrasive disk space is 1-30 μ m.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417682A (en) * | 2011-09-29 | 2012-04-18 | 浙江农林大学 | High tensile strength multicomponent mixed inclusion PVB (polyvinyl butyral) diaphragm and production method thereof |
| US20150308017A1 (en) * | 2012-11-09 | 2015-10-29 | Stora Enso Oyj | Mixing drying of nanofibrillated polysaccharide |
| CN105568728A (en) * | 2015-12-03 | 2016-05-11 | 雷春生 | Method for preparing nanocellulose from Urtica fissa stalks |
| CN107936301A (en) * | 2017-11-07 | 2018-04-20 | 嘉兴学院 | A kind of bacterial fibers film with dendritic structure and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101818467A (en) * | 2010-03-29 | 2010-09-01 | 南京林业大学 | Method for manufacturing cellulose micro-nano-material enhanced adhesive by using enzyme treatment and mechanical method |
| CN101864606A (en) * | 2010-06-30 | 2010-10-20 | 东北林业大学 | Preparation method of biomass cellulose nanofibers with high length-diameter ratio |
-
2011
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101818467A (en) * | 2010-03-29 | 2010-09-01 | 南京林业大学 | Method for manufacturing cellulose micro-nano-material enhanced adhesive by using enzyme treatment and mechanical method |
| CN101864606A (en) * | 2010-06-30 | 2010-10-20 | 东北林业大学 | Preparation method of biomass cellulose nanofibers with high length-diameter ratio |
Non-Patent Citations (2)
| Title |
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| SAITO T.等: "TEMPO-Mediated Oxidation of Native Cellulose.The Effect of Oxidation Conditions on Chemical and Crystal Structures of the Water-Insoluble Fractions.", 《BIOMACROMOLECULES》 * |
| 董硕等: "酵母菌产纤维素酶的发酵条件研究", 《饲料研究》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417682A (en) * | 2011-09-29 | 2012-04-18 | 浙江农林大学 | High tensile strength multicomponent mixed inclusion PVB (polyvinyl butyral) diaphragm and production method thereof |
| US20150308017A1 (en) * | 2012-11-09 | 2015-10-29 | Stora Enso Oyj | Mixing drying of nanofibrillated polysaccharide |
| CN105568728A (en) * | 2015-12-03 | 2016-05-11 | 雷春生 | Method for preparing nanocellulose from Urtica fissa stalks |
| CN107936301A (en) * | 2017-11-07 | 2018-04-20 | 嘉兴学院 | A kind of bacterial fibers film with dendritic structure and preparation method thereof |
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Application publication date: 20110907 |