CN106928374A - A kind of preparation method of Cactaeous plants needle Cellulose nanocrystal palpus - Google Patents
A kind of preparation method of Cactaeous plants needle Cellulose nanocrystal palpus Download PDFInfo
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- CN106928374A CN106928374A CN201710173202.XA CN201710173202A CN106928374A CN 106928374 A CN106928374 A CN 106928374A CN 201710173202 A CN201710173202 A CN 201710173202A CN 106928374 A CN106928374 A CN 106928374A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
Abstract
The present invention relates to a kind of preparation method of Cactaeous plants needle Cellulose nanocrystal palpus, belong to biomass-based technical field of material.Preparation method of the invention, including alkali process, dried process, DES treatment and homogenization step；Wherein, the DES, is according to 2 by Choline Chloride and organic acid:The supernatant liquid that 16 mixed in molar ratio is obtained after 50 DEG C of 160 DEG C of constant temperature；In homogenization, the pressure of high pressure Microfluidizer used is 1100 2300bar.The present invention has successfully prepared Cellulose nanocrystal palpus as raw material with the needle of Cactaeous plants first；Cactaeous plants leaf thorn aboundresources, the low cost for being used, both solve problem of environmental pollution, and the added value of Cactaeous plants needle is improve again.The present invention is in preparation process using DES treatment, it is to avoid the purification by liquid extraction step of cumbersome nano-cellulose whisker, reduce production cost, it is to avoid environmental pollution.
Description
Technical field
The present invention relates to a kind of preparation method of Cactaeous plants needle Cellulose nanocrystal palpus, belong to biomass base material
Material preparing technical field.
Background technology
Natural long through a class that esterification is generated by 1,4- beta-glucosidases by β-D- glucose sugar unit of cellulose
Chain compound, it is widely present in nature, and the length of its chain is very different, and the glucose unit in molecule is from hundreds of
Individual to contain free oh group in the sugar unit for constantly repeating to more than 30,000, the hydroxyl in adjacent chain can pass through
Hydrogen bond is combined and expands crystal region, and these crystal regions exist in the form of pencil or laminar cellulose microfibril, in order
The cellulose crystallite of nanoscale microfibril or nanowhisker the formation rule arrangement of arrangement, and disorderly arranged then foring is unformed
Hemicellulose matrix.At present, cellulose nanowhisker can be extracted from cellulose nanometer fibril by acid-hydrolyzed method, one
Under fixed control condition, the product of cellulose can be improved by the amorphous region around hydrolyzing and embedded cellulose fibril
Amount.
In order to reduce environmental pollution and and its harm to environment for human survival, the biomass-based chemical combination of people's numerous studies
The research of thing material, to seek technology and environmentally friendly product, how using nature be widely present can
Regenerated resources become a kind of new research field obtaining biomass compound.Cellulose nanocrystal must be from many kinds certainly
Obtained in right plant or Animal resources, such as beans, cotton, banana, shell, coconut husk, stalk, the fibre proposed from these resources
The plain nano whisker of dimension can be used to improve as the biological filler agent of many compounds the performance of target compound.At present, from certainly
The method and step of extraction Cellulose nanocrystal palpus is in right plant：Again through sour water solution after biochemistry pretreatment, then by cumbersome
The steps such as extraction, purification, can just obtain nanofiber whisker.
Cactaeous plants are planted and cultivated in Guangdong Province of China, Fujian Province extensively, remove the leaf of needle prick shape（Needle）Afterwards
Can be used to keep fowls；But, currently without on preparing Cellulose nanocrystal by raw material of the needle of Cactaeous plants
The relevant report of palpus.
The content of the invention
It is an object of the invention to provide a kind of needle with Cactaeous plants Cellulose nanocrystal palpus is prepared as raw material
Method.
The present invention is achieved by the following technical solutions：
A kind of preparation method of Cactaeous plants needle Cellulose nanocrystal palpus, comprises the following steps：
（1）Alkali process：The needle of Cactaeous plants is placed in aqueous slkali, 90-150min is stirred in 70-90 DEG C, collected not
Molten thing；
（2）Dried process：The pH of insoluble matter is adjusted to 6.5-7.5, is then dried, obtain A；
（3）DES treatment：A is added in DES, is processed 2-10 hours in 50-160 DEG C, be subsequently adding cold water cooling and be quenched, obtained
To DES-A；The cold water refers to less than 10 DEG C of water；The DES, is according to 2 by Choline Chloride and organic acid:1-6 mole
Than mixing the supernatant liquid obtained after 50 DEG C of -160 DEG C of constant temperature；The mass ratio of DES and A is 1:54-1000；
（4）Homogenization：The pH value of DES-A is adjusted to 6.5-7.5, plus deionized water is made into suspension B, loads high after homogeneous
Pressure Microfluidizer is processed；The weight/mass percentage composition of DES-A is 0.1-2.2%, high pressure microjet in suspension B
Homogenizer pressure is 1100-2300bar.
Above-mentioned preparation method, it is preferred that the alkali process of step 1 are：The needle of Cactaeous plants is placed in mass concentration
It is 10% sodium hydrate aqueous solution, 120min is stirred in 80 DEG C；The needle of Cactaeous plants and the hydrogen that mass concentration is 10%
The mass ratio of aqueous solution of sodium oxide is 1:0.5-3.6；It is furthermore preferred that the needle of Cactaeous plants and mass concentration are 10%
The mass ratio of sodium hydrate aqueous solution is 1:2.
Above-mentioned preparation method, it is preferred that the dried process of step 2 is：The pH of insoluble matter is adjusted to 7, then in 60 DEG C
24h is dried, A is obtained.
Above-mentioned preparation method, it is preferred that the process time of step 3 is 2-4 hours；In step 3, the mass ratio 1 of DES and A：
100, the cold water of addition is 1 with the mass ratio of A：50-350.
Above-mentioned preparation method, the organic acid in DES used by step 3 can be to a hydration p-methyl benzenesulfonic acid, anhydrous to first
One kind in benzene sulfonic acid, anhydrous oxalic acid, two oxalic acid hydrates and levulic acid；
Preferably to a hydration toluenesulfonic acid, now treatment temperature is 60 DEG C；
When organic acid is anhydrous p-methyl benzenesulfonic acid, anhydrous oxalic acid, two oxalic acid hydrates or levulic acid, treatment temperature is 120 DEG C；
When organic acid is anhydrous oxalic acid, levulic acid, the molar ratio of Choline Chloride and organic acid is 1:2；
When organic acid be two oxalic acid hydrates, to a hydration p-methyl benzenesulfonic acid, anhydrous p-methyl benzenesulfonic acid when, Choline Chloride and organic acid
Molar ratio be 1:1.
Above-mentioned preparation method, it is preferred that in step 4, the weight/mass percentage composition of DES-A is 0.5% in suspension B, during homogeneous
Rotating speed be 6000rpm-15000rpm, high pressure Microfluidizer pressure be 2000bar, the bin of high pressure Microfluidizer
Aperture is 60-40 μm.
Relative to the existing method for preparing Cellulose nanocrystal palpus as raw material with plant, the improvement of preparation method of the invention
Part is using DES treatment, while to coordinate DES treatment, increased dried process before DES treatment, processing it in DES
After increased homogenization.The present invention is first processed for preparing Cellulose nanocrystal palpus technical field, at DES DES
Reason only needs a step to process and can obtain Cellulose nanocrystal beam, instead of cumbersome extraction, purification in existing preparation method etc. and walks
Suddenly, production cost is reduced, it is to avoid environmental pollution.
Preparation method of the invention, the treatment temperature of step 3, the concentration of the suspension B of step 4, high pressure microjet homogeneous
Machine pressure is the key parameter for successfully preparing Cellulose nanocrystal palpus；Scope is limited beyond the present invention, then cannot obtain fiber
Plain nano whisker, but obtain Cellulose nanocrystal beam or Cellulose nanocrystal.
In the present invention, " needles of Cactaeous plants " refer to the leaf of the needle prick shape of Cactaeous plants；The celestial being
Palm section plant can be one or more in cactus, celestial being's post and cactus with globular.
Beneficial effect：
The present invention has successfully prepared Cellulose nanocrystal palpus as raw material with the needle of Cactaeous plants first；The celestial being for being used
Leaf aboundresources, the low cost of Ren Zhang sections plant needle prick shape, both solve problem of environmental pollution, and Cactaceae plant is improve again
The added value of thing needle.The present invention is in preparation process using DES treatment, it is to avoid the extraction of cumbersome nano-cellulose whisker
Purification step, reduce production cost, it is to avoid environmental pollution.
Specific embodiment
With reference to specific embodiment, the invention will be further described；Except as otherwise indicating, the number in embodiment
It is by weight.
Embodiment 1
The pretreatment of needle：By 1 part of cactus with globular needle（Take from Zhangzhou, Fujian, needle length 2cm）It is placed in 10 parts of ethanol waters
In wash away impurity, be subsequently placed in baking oven and dried at 60 DEG C, then distribute it to 0.5 part of concentration（Mass concentration, similarly hereinafter）For
In 10% sodium hydrate aqueous solution, stirred in 80 DEG C 2 hours, then by washing, filtering, the solid product that will be obtained adds water
After dispersion, it is 7 to be titrated to pH with the acetum of 1mol/L, and finally drying obtains solid product A in 24 hours at 60 DEG C；
DES treatment：By Choline Chloride and a hydration p-methyl benzenesulfonic acid in molar ratio 1：3 mixing, 30 points of stir process at 60 DEG C
Clock obtains the DES of supernatant liquid shape, 1 part of A is added directly into 1000 parts of DES is uniformly dispersed at once, keeps the temperature to continue
Heating 4 hours, is subsequently adding 50 parts of cold water coolings and is quenched, and obtains DES-A；The yield of DES-A is 76%,（Yield=(DES-A/
A) * 100%, similarly hereinafter）；
Washing and decentralized processing：DES-A is washed with deionized and filters, and is then adjusted to 7 its pH value with NaOH,
Plus deionized water is made into the suspension B that mass fraction is 0.1%；B loading homogenizers are stirred evenly under 6000rpm, height is then charged into
Pressure Microfluidizer, is obtained Cactaeous plants needle Cellulose nanocrystal in 1100bar pressure, 60 μm of aperture bins
Palpus；Whisker width 11nm, length 660nm, crystallinity index (CrIs) 70%, carbonyl content 0.24mmol/g, good thermal stability
（290 DEG C take place thermal degradation）.
Embodiment 2
The pretreatment of needle：By 1 part of cactus needle（Take from Hui nationality, needle length 7cm）It is placed in 20 parts of ethanol waters
In, impurity is washed away, it is subsequently placed in baking oven and is dried at 60 DEG C, then distributes it to the sodium hydrate aqueous solution that 2 parts of concentration is 10%
In, in being stirred at 80 DEG C 2 hours, then by washing, filtering, the solid product that will be obtained adds water after dispersion, with 1mol/L's
It is 7 that acetum is titrated to pH, and finally drying obtains solid product A in 24 hours at 60 DEG C；
DES treatment：By Choline Chloride and anhydrous p-methyl benzenesulfonic acid in molar ratio 1：2 mixing, stir stir process 30 at 50 DEG C
Minute obtains the DES of supernatant liquid shape, 1 part of A is added directly into 54 parts of DES is uniformly dispersed at once, keeps the temperature to continue
Heat 10 hours, be subsequently adding 350 parts of cold water coolings and be quenched, obtain DES-A；The yield of DES-A is 71%；
Washing and decentralized processing：DES-A is washed with deionized and filters, and is then adjusted to 7 its pH value with NaOH,
Plus deionized water is made into the suspension B that mass fraction is 2.2%；B loading homogenizers are stirred evenly under 15000rpm, is then charged into
High pressure Microfluidizer, is obtained Cactaeous plants needle cellulose nanometer in 2000bar pressure, 400 μm of aperture bins
Whisker；Whisker width 19nm, length 573nm, crystallinity index (CrIs) 68.2%, carbonyl content 0.21mol/Lmol/g, heat are steady
It is qualitative good（278 DEG C take place thermal degradation）.
Embodiment 3
The pretreatment of needle：By 1 part of celestial being's post needle（Take from East China, needle length 18cm）It is placed in 35 parts of ethanol waters
In wash away impurity, be subsequently placed in baking oven and dried at 60 DEG C, then distribute it to the NaOH water that 3.6 parts of concentration is 10%
In solution, in being stirred at 80 DEG C 2 hours, then by washing, filtering, the solid product that will be obtained adds water after dispersion, uses 1mol/
The acetimetry of L is 7 to pH, and finally drying obtains solid product A in 24 hours at 60 DEG C；
DES treatment：By Choline Chloride and levulic acid in molar ratio 1：2 mixing, stir process obtains clear in 30 minutes at 120 DEG C
, be added directly into 1 part of A in 100 parts of DES be uniformly dispersed at once by clear liquid DES, keeps the temperature to continue to heat 4
Hour, it is subsequently adding 100 parts of cold water coolings and is quenched, obtain DES-A；The yield of DES-A is 75%；
Washing and decentralized processing：DES-A is washed with deionized and filters, and is then adjusted to 7 pH value with NaOH, plus
Deionized water is made into the suspension B that mass fraction is 0.5%, and B loading homogenizers are stirred evenly under 11000rpm, is then charged into height
Pressure Microfluidizer, is obtained Cactaeous plants needle Cellulose nanocrystal in 2000bar pressure, 80 μm of aperture bins
Palpus；Whisker width 7nm, length 723nm, crystallinity index (CrIs) 72.2%, carbonyl content 0.28mmol/g, heat endurance is good
It is good（283 DEG C take place thermal degradation）.
Embodiment 4
The pretreatment of needle：By 1 part of celestial being's post needle（Take from East China, needle length 18cm）It is placed in 35 parts of ethanol waters
In wash away impurity, be subsequently placed in baking oven and dried at 60 DEG C, then distribute it to the NaOH water that 3.6 parts of concentration is 10%
In solution, in being stirred at 80 DEG C 2 hours, then by washing, filtering, the solid product that will be obtained adds water after dispersion, uses 1mol/
The acetimetry of L is 7 to pH, and finally drying obtains solid product A in 24 hours at 60 DEG C；
DES treatment：By Choline Chloride and two oxalic acid hydrates in molar ratio 2：1 mixing, stir process is obtained for 30 minutes at 120 DEG C
, be added directly into 1 part of A in 200 parts of DES be uniformly dispersed at once by the DES of supernatant liquid shape, keeps the temperature to continue to heat
6 hours, it is subsequently adding 200 parts of cold water coolings and is quenched, obtains DES-A；The yield of DES-A is 69%；
Washing and decentralized processing：DES-A is washed with deionized and filters, and is then adjusted to 7 pH value with NaOH, plus
Deionized water is made into the suspension B that mass fraction is 1.5%, and B loading homogenizers are stirred evenly under 12000rpm, is then charged into height
Pressure Microfluidizer, is obtained Cactaeous plants needle Cellulose nanocrystal in 1700bar pressure, 87 μm of aperture bins
Palpus；Whisker width 12nm, length 611nm, crystallinity index (CrIs) 67.2%, carbonyl content 0.2mmol/g, heat endurance is good
It is good（277 DEG C take place thermal degradation）.
Embodiment 5
The pretreatment of needle：By 1 part of celestial being's post needle（Take from East China, needle length 18cm）It is placed in 35 parts of ethanol waters
In, impurity is washed away, it is subsequently placed in baking oven and is dried at 60 DEG C, then distributes it to the NaOH water that 3.6 parts of concentration is 10%
In solution, in being stirred at 80 DEG C 2 hours, then by washing, filtering, the solid product that will be obtained adds water after dispersion, uses 1mol/
The acetimetry of L is 7 to pH, and finally drying obtains solid product A in 24 hours at 60 DEG C；
DES treatment：By Choline Chloride and anhydrous oxalic acid in molar ratio 1：1 mixing, stir process obtains clear in 30 minutes at 120 DEG C
, be added directly into 1 part of A in 250 parts of DES be uniformly dispersed at once by clear liquid DES, keeps the temperature to continue to heat 7
Hour, it is subsequently adding 280 parts of cold water coolings and is quenched, obtain DES-A；The yield of DES-A is 72%；
Washing and decentralized processing：DES-A is washed with deionized and filters, and is then adjusted to 7 pH value with NaOH, plus
Deionized water is made into the suspension B that mass fraction is 1%, and B loading homogenizers are stirred evenly under 15000rpm, is then charged into high pressure
Microfluidizer, is obtained Cactaeous plants needle Cellulose nanocrystal palpus in 2000bar pressure, 100 μm of aperture bins；
Whisker width 14nm, length 573nm, crystallinity index (CrIs) 71.1%, carbonyl content 0.26mmol/g, good thermal stability
（297 DEG C take place thermal degradation）.
Claims (9)
1. a kind of Cactaeous plants needle Cellulose nanocrystal must preparation method, it is characterised in that comprise the following steps：
（1）Alkali process：The needle of Cactaeous plants is placed in aqueous slkali, 90-150min is stirred in 70-90 DEG C, collected not
Molten thing；
（2）Dried process：The pH of insoluble matter is adjusted to 6.5-7.5, is then dried, obtain A；
（3）DES treatment：A is added in DES, is processed 2-10 hours in 50-160 DEG C, be subsequently adding cold water cooling and be quenched, obtained
To DES-A；The cold water refers to less than 10 DEG C of water；The DES, is according to 2 by Choline Chloride and organic acid:1-6 mole
Than mixing the supernatant liquid obtained after 50 DEG C of -160 DEG C of constant temperature；The mass ratio of DES and A is 1:54-1000；
（4）Homogenization：The pH value of DES-A is adjusted to 6.5-7.5, plus deionized water is made into suspension B, loads high after homogeneous
Pressure Microfluidizer is processed；The weight/mass percentage composition of DES-A is 0.1-2.2%, high pressure microjet in suspension B
Homogenizer pressure is 1100-2300bar.
2. preparation method according to claim 1, it is characterised in that the alkali process of step 1 are：By Cactaeous plants
Needle is placed in the sodium hydrate aqueous solution that mass concentration is 10%, and 120min is stirred in 80 DEG C；The needle and matter of Cactaeous plants
Amount concentration is that the mass ratio of 10% sodium hydrate aqueous solution is 1:0.5-3.6.
3. preparation method according to claim 2, it is characterised in that the needle of Cactaeous plants is with mass concentration
The mass ratio of 10% sodium hydrate aqueous solution is 1:2.
4. the preparation method according to claim 1,2 or 3, it is characterised in that the dried process of step 2 is：By insoluble matter
PH be adjusted to 7, then dry 24h in 60 DEG C, obtain A.
5. preparation method according to claim 4, it is characterised in that the process time of step 3 is 2-4 hours；Step 3
In, the mass ratio 1 of DES and A：100, the cold water of addition is 1 with the mass ratio of A：50-350.
6. preparation method according to claim 5, it is characterised in that the organic acid in DES used by step 3 is to a hydration
One kind in p-methyl benzenesulfonic acid, anhydrous p-methyl benzenesulfonic acid, anhydrous oxalic acid, two oxalic acid hydrates and levulic acid.
7. preparation method according to claim 6, it is characterised in that the organic acid in DES used by step 3 is to a hydration
During toluenesulfonic acid, treatment temperature is 60 DEG C；Organic acid in DES used by step 3 is anhydrous p-methyl benzenesulfonic acid, anhydrous oxalic acid, two
When oxalic acid hydrate or levulic acid, treatment temperature is 120 DEG C.
8. preparation method according to claim 7, it is characterised in that the organic acid in DES used by step 3 is without pasture and water
When acid, levulic acid, the molar ratio of Choline Chloride and organic acid is 1:2；Organic acid in DES used by step 3 is two hydrations
Oxalic acid, to one hydration p-methyl benzenesulfonic acid, anhydrous p-methyl benzenesulfonic acid when, the molar ratio of Choline Chloride and organic acid is 1:1.
9. preparation method according to claim 8, it is characterised in that in step 4, the quality percentage of DES-A in suspension B
Content is 0.5%, and rotating speed during homogeneous is 6000rpm-15000rpm, and high pressure Microfluidizer pressure is 2000bar, high pressure
The bin aperture of Microfluidizer is 60-40 μm.
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| CN107815911A (en) * | 2017-09-18 | 2018-03-20 | 浙江纺织服装职业技术学院 | A kind of preparation method of nano-cellulose fibril |
| CN109235102A (en) * | 2018-10-25 | 2019-01-18 | 齐鲁工业大学 | A kind of method of eutectic solvent pretreatment preparation cellulose nanometer fibril |
| CN111187356A (en) * | 2020-03-25 | 2020-05-22 | 齐鲁工业大学 | Method for preparing microcrystalline cellulose by treating poplar wood powder with eutectic solvent and acid |
| WO2022027150A1 (en) * | 2020-08-07 | 2022-02-10 | Pontificia Universidad Católica De Chile | Method for preparing nanocellulose using specially synthesised "green" solvents |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107815911A (en) * | 2017-09-18 | 2018-03-20 | 浙江纺织服装职业技术学院 | A kind of preparation method of nano-cellulose fibril |
| CN109235102A (en) * | 2018-10-25 | 2019-01-18 | 齐鲁工业大学 | A kind of method of eutectic solvent pretreatment preparation cellulose nanometer fibril |
| CN109235102B (en) * | 2018-10-25 | 2021-01-08 | 齐鲁工业大学 | Method for preparing cellulose nanofibrils through pretreatment of eutectic solvent |
| CN111187356A (en) * | 2020-03-25 | 2020-05-22 | 齐鲁工业大学 | Method for preparing microcrystalline cellulose by treating poplar wood powder with eutectic solvent and acid |
| WO2022027150A1 (en) * | 2020-08-07 | 2022-02-10 | Pontificia Universidad Católica De Chile | Method for preparing nanocellulose using specially synthesised "green" solvents |
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