CN106279440A - A kind of preparation method of carboxyethylation modified Nano fibrillated fibers element - Google Patents
A kind of preparation method of carboxyethylation modified Nano fibrillated fibers element Download PDFInfo
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- CN106279440A CN106279440A CN201510268190.XA CN201510268190A CN106279440A CN 106279440 A CN106279440 A CN 106279440A CN 201510268190 A CN201510268190 A CN 201510268190A CN 106279440 A CN106279440 A CN 106279440A
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Abstract
The preparation method of a kind of carboxyethylation modified Nano fibrillated fibers element, it relates to the preparation method of a kind of nano-cellulose.Method: the sodium hydroxide solution first with excess carries out alkali swelling treatment to cellulose paste, it is subsequently adding a certain amount of acrylamide solution to be modified, after reaction a period of time at a certain temperature, wash and filter, obtain carboxyethylation cellulose, finally utilize the mechanization shearing equipments such as high pressure homogenizer that carboxyethylation cellulose machinery fibrillation is processed, obtain stable Nanowire cellulose suspension.Inventive process avoids and environment causes acid pollution, and preparation method is simple, overcomes the problem that nanofiber procatarxis hydrogen bond is easily reunited, the diameter of the carboxyethylation modified nanometer cellulose obtained is less than 50nm, and transparency is high, good stability.
Description
Technical field
The present invention relates to the preparation method of a kind of nano-cellulose, belong to technical field of nano material.
Background technology
Nano-cellulose particularity on aggregated structure with physical property so that it is at barrier coating, food, cosmetics, papermaking and biology
The industrial fields such as medical material, energy storage material, filtering material, high-performance composite materials have broad application prospects.
The method preparing nano-cellulose has chemical method (acid-hydrolysis method), physicomechanical processes, bioanalysis, (chemical/biological) pretreatment to combine
Mechanical treatment process etc..
Use nano-cellulose prepared by mineral acid hydrolysis method, although the nano-cellulose obtained has preferable dispersibility and stability,
But reaction system can remaining substantial amounts of acid and impurity, need to consume substantial amounts of water and power source to obtain nano-cellulose,
Improve preparation cost, and environment is easily caused acid pollution by the sewage of discharge, the most existing mineral acid hydrolysis method prepares nanofiber
It is high to there is cost in element method, the easily problem to environment.
Fully utilized physical mechanical processes the mode of cellulose can prepare nano-cellulose.Such as, US 4374702 discloses one and receives
The preparation method of rice cellulose, is to utilize high pressure homogenizer to make cellulose suspension lead under conditions of at least 3000psig pressure drop
Crossing the homogenizing valve of small gap, cellulose, by mechanisms such as strong impact and shearings, finally dissociates and becomes diameter
The nano-cellulose of 25nm～100nm.The method is that the most fully utilized mechanism prepares nano-cellulose, but,
This preparation method needs to consume substantial amounts of energy, and preparation cost is high, and the easy occluding device of cellulose suspension, impact preparation effect
Rate.
In order to reduce the preparation energy consumption of nano-cellulose, a lot of methods consider cellulose is carried out pretreatment.
US 20090221812 discloses the preparation method of a kind of nano-cellulose, is first to pull an oar cellulose, is subsequently adding list
Component glucose restriction endonuclease processes, and finally homogenize process to cellulose, prepares the nanofiber of a diameter of 3.5nm～18nm
Element.Comparing the energy expenditure of US 4374702 method (cellulose not being carried out pretreatment), the energy expenditure of the method at least drops
Low by 80%.US 20110036522 discloses the preparation method of a kind of nano-cellulose, is first with the both sexes containing electrolyte
Cellulose derivative aqueous solution to fiber material modification pretreatment, then mechanical treatment, obtain the MFC hydrogel that transparency is high.
The method compares the energy expenditure of US 4374702 method, reduces 98%, and avoids fiber blocking plant equipment.Non-patent
Document: (1) " TEMPO-Mediated Oxidation of Native Cellulose.The Effect of Oxidation
Conditions on Chemical and Crystal Structures of the Water-Insoluble Fractions”.
Tsuguyuki Saito, Akira Isogai.Biomacromolecules.2004,5 (5): 1983-1989. (2)
" TEMPO-oxidized cellulose nanofibers " .Akira Isogai, Tsuguyuki Saito, Hayaka Fukuzumi.
Nanoscale, 2011,3 (1): 71-85. describe native cellulose is carried out TEMPO (2,2,6,6-tetramethyl piperidine nitrogens oxidation
Thing) induced oxidation pretreatment, the C6 position primary hydroxyl of cellulose will optionally be oxidized to carboxyl, the cellulose carboxyl after oxidation
Content is 0.5mmol/g～2.5mmol/g, then carries out mechanical treatment, has obtained the fibre diameter nano-cellulose less than 50nm
Water slurry.Along with the raising of cellulose carboxyl-content, the energy consumption of mechanical treatment is also greatly reduced.CN 102443067
Disclose the preparation method of a kind of carboxide modified nanometre cellulose, fine to dried crystallite first with anhydrous dimethyl sulphoxide
Dimension element carries out swelling, secondly uses thionyl chloride to carry out nanorize process, then passes to ammonia and be modified, and remove impurity,
Under ultrasonic assistant, obtain stable nano-cellulose suspension, the most freeze-dried i.e. obtain carbonylation modified nano fiber
Element.But said method all uses Organic substance as reaction medicine, and preparation cost is high, and carrying capacity of environment is big.
Having the manufacture method of carboxyethyl modified cellulose in the prior art, such as, US20060137838 discloses and is using corresponding chlorine alkane
Acid as reaction reagent under conditions of, with carboxymethyl cellulose the same manner by pulp production carboxyethyl cellulose.The method ten
Divide the production of applicable carboxymethyl cellulose, but it is but the most infeasible for producing carboxyethyl cellulose the most similarly.
US5667637 discloses and is prepared carboxyethylcellulose with polymine, cationic starch with polyene acyl-epichlorohydrin resins by paper pulp
Element, can improve pop strength and the deflection of paper in papermaking is applied.CN 102471940 disclose carboxyethylcellulose cellulose fiber,
Its application in Wound bandage and hygienic articles and manufacture method, the preparation of the most water-fast carboxyethylcellulose cellulose fiber
Method, is to make cellulose staple fibre and acrylamide react in the aqueous alkali that concentration is 2%～10%, the most again uses concentration
It it is alkali liquor (comprising the ethanol of the 1%～75% weight) post processing of 3%～10%.Wherein use laser that as cellulose staple fibre
Fiber, viscose rayon or Modal fibre, the carboxyethylcellulose cellulose fiber of manufacture is for Wound bandage and other medical usage.But
Above-mentioned preparation method uses Organic substance to be reaction medium, and flow process is relatively cumbersome, and has not yet to see the system being applied to nano-cellulose
In Preparation Method.
Summary of the invention
The present invention does not use mineral acid hydrolysis, there is not the acid of remaining, it is to avoid easily cause acid pollution to ask environment in reaction system
Topic；Secondly, preparation method of the present invention is simple, and avoids consuming substantial amounts of water and power source because reaction system concentration is high,
Cellulose modified rear carboxyethyl content is high, beneficially the dissociating and reduce the energy consumption that machinery fibrillation processes of fiber, and preparation cost obtains
To be greatly reduced；Easily reunite it addition, carboxyethylation modified nanometer cellulose prepared by the present invention overcomes nanofiber procatarxis hydrogen bond
Problem, be distributed to the most uniformly aqueous systems, ethanol system, starch system, polyvinyl alcohol system, acrylic resin systems,
In DMF (DMF) system, expand the range of application of nano-cellulose, and carboxyethyl prepared by the present invention
Changing modified nanometer cellulose good stability, therefore carboxyethylation modified nanometer cellulose the aspect such as is prepared at new material and is had good
Application prospect.
The present invention provides the preparation method of the carboxyethylation modified Nano fibrillated fibers element of a kind of simplicity.Wherein, carboxyethyl modification is to utilize
Following reaction principle realizes:
There is additive reaction in the basic conditions in cellulose and acrylamide, generates carbamyl ethyl cellulose, see reaction equation (1)；First
Aminoacyl ethyl cellulose hydrolyzes under heating and alkaline environment, generates sodium hydroxyethlcellulose and ammonia, sees reaction equation (2).
The preparation method of a kind of carboxyethylation modified Nano fibrillated fibers element, is specifically realized by the following steps:
One, get the raw materials ready: weigh a certain amount of pulpboard, be torn into fractionlet shape or be ground to powder, standby.Pulpboard includes leaf wood herein
Pulpboard, needlebush pulpboard, pulp plate, cotton starch plate, bamboo pulp plate, reed pulp plate, jute pulp plate and agricultural crop straw pulpboard, or phase
The wet pulp answered, but it is not limited only to this；
Two, alkali swollen processes: adds the NaOH solution that 5%～200% (relative to fibrous raw material) mass concentration is 10%～30% and makes
The abundant swollen of fiber, processes 8h～24h；
Three, carboxyethylation is modified: fibre stuff is concentrated into finite concentration, then is added thereto to 5%～200% (relative to fibrous raw material)
Mass concentration is the acrylamide aqueous solution of 5%～50%, controls reaction temperature 60 DEG C～90 DEG C, reaction 2h～6h, be washed out,
Filter, obtain carboxyethylation cellulose suspension；Modified carboxyethyl content is 0.5mmol/g～2.5mmol/g；
Four, nanofibrilsization processes: with high pressure homogenizer, the carboxyethyl cellulose suspension under 1%～4% concentration is carried out mechanization process,
I.e. obtaining stable carboxyethylation Nanowire cellulose, a diameter of 5nm～100nm, length 0.5 μm～10 μm, 0.1% is dense
The carboxyethylation Nanowire cellulose suspension under Du transmitance under 500nm wavelength is 72%～82%, 660nm wavelength
Under transmitance be 75%～85%；Wherein, high pressure homogenizer also includes microfluidizer, or uses fine grinding machine, food to add
Work machine etc., but it is not limited only to this.
Inventive process avoids and environment is caused acid pollution, and preparation method is simple, overcomes what nanofiber procatarxis hydrogen bond was easily reunited
Problem, the diameter of the carboxyethylation modified nanometer cellulose obtained is less than 50nm, and transparency is high, good stability.
Detailed description of the invention
Present embodiment is the preparation method of a kind of carboxyethylation modified nanometer cellulose,
Below by embodiment, the present invention will be further described
Embodiment 1: weigh 20g leaf wood pulpboard (being equivalent to 18.86g oven-dry weight), be torn into fractionlet and be dispersed as powder；Add
5-200% (relative to fibrous raw material) mass concentration be 20% NaOH solution make the abundant swollen of fiber, process 24h；Extruding
Being concentrated into 180g, the another 200mL mass concentration that adds is the acrylamide solution of 20%, it is ensured that overall reaction system slurry is dense is 5%；
Controlling modified-reaction temperature with hot bath is 90 DEG C, reacts 5h, is washed out, filters, obtain carboxyethylation cellulose, surveys
The carboxyethyl content measuring this carboxyethylation modified cellulose is 1.28mmol/g；Carboxyethylation cellulose suspension is diluted to 1%
Concentration, carries out homogenizing, nanofibrilsization process with high pressure homogenizer to it, finally gives carboxyethylation Nanowire cellulose.
The carboxyethylation Nanowire cellulose suspension under 0.1% concentration is measured at 500nm wavelength with ultra-violet and visible spectrophotometer
Under transmitance be 74.59%；Transmitance under 660nm wavelength is 75.07%；Measure with transmission electron microscope(TEM) (TEM)
The diameter of carboxyethylation Nanowire cellulose is about 100nm, and length is about 5 μm.
Embodiment 2: weigh 20g leaf wood pulpboard (being equivalent to 18.86g oven-dry weight), be torn into fractionlet and be dispersed as powder；Add
5-200% (relative to fibrous raw material) mass concentration be 20% NaOH solution make the abundant swollen of fiber, process 24h；Add
5-200% (relative to fibrous raw material) mass concentration is the acrylamide solution of 20%, is concentrated into 153.84g, really after stirring
Protecting overall reaction system slurry dense is 13%；Controlling modified-reaction temperature with hot bath is 70 DEG C, reacts 3h, is washed out, filters,
Obtaining carboxyethylation cellulose, the carboxyethyl content measuring this carboxyethylation modified cellulose is 1.69mmol/g；By carboxyethylation
Cellulose suspension is diluted to 1% concentration, with high pressure homogenizer, it is carried out homogenizing, nanofibrilsization process, finally gives carboxylic second
Base Nanowire cellulose.The carboxyethylation Nanowire cellulose under 0.1% concentration is measured with ultra-violet and visible spectrophotometer
Suspension transmitance under 500nm wavelength is 70.67%；Transmitance under 660nm wavelength is 75.59%；Use electronic transmission
Microscope (TEM) is measured the diameter of carboxyethylation Nanowire cellulose and is about 50nm, and length is about 4 μm.
Embodiment 3: weigh 20g leaf wood pulpboard (being equivalent to 18.86g oven-dry weight), be torn into fractionlet and be dispersed as powder；Add
5-200% (relative to fibrous raw material) mass concentration be 20% NaOH solution make the abundant swollen of fiber, process 24h；Extruding
Concentrating the fibre stuff after alkali swollen, make slurry concentration 31.73%, the another 15mL mass concentration that adds is the acrylamide of 20%
Solution, it is ensured that overall reaction system slurry is dense is 24%；Controlling modified-reaction temperature with hot bath is 70 DEG C, reacts 3h, then washes
Washing, filter, obtain carboxyethylation cellulose, the carboxyethyl content measuring this carboxyethylation modified cellulose is 1.89mmol/g；
Carboxyethylation cellulose suspension is diluted to 1% concentration, with high pressure homogenizer, it is carried out homogenizing, nanofibrilsization process,
Obtain carboxyethylation Nanowire cellulose eventually.The carboxyethylation nanometer under 0.1% concentration is measured with ultra-violet and visible spectrophotometer
Fibrillated fibers element suspension transmitance under 500nm wavelength is 80.75%；Transmitance under 660nm wavelength is 83.35%；
The diameter measuring carboxyethylation Nanowire cellulose with transmission electron microscope(TEM) (TEM) is about 20nm, and length is about 1.5 μ
m。
Claims (10)
1. the preparation method of a carboxyethylation modified Nano fibrillated fibers element, it is characterised in that carboxyethylation modified Nano fibrillated fibers
The preparation method of element completes according to the following steps: one, gets the raw materials ready: weigh a certain amount of pulpboard, is torn into fractionlet shape or is ground to
Powder, standby；Two, alkali swollen processes: adds certain density NaOH solution in fibrous raw material and makes the abundant swollen of fiber,
Process a period of time；Three, carboxyethylation is modified: fibre stuff is concentrated into finite concentration, then is added thereto to certain density
Acrylamide aqueous solution, controls reaction temperature and response time, completes carboxyethyl modifying process；Four, nanofibrilsization processes:
The aforementioned carboxyethylation cellulose suspension obtained carries out mechanical shearing, nanofibrilsization processes, and finally gives carboxyethylation and receives
Rice fibrillated fibers element.
The preparation method of a kind of carboxyethylation modified Nano fibrillated fibers the most according to claim 1 element, it is characterised in that pulpboard bag
Include leaf wood pulpboard, needlebush pulpboard, pulp plate, cotton starch plate, bamboo pulp plate, reed pulp plate, jute pulp plate and agricultural crop straw slurry
Plate, or corresponding wet pulp, but it is not limited only to this.
The preparation method of a kind of carboxyethylation modified Nano fibrillated fibers the most according to claim 1 element, it is characterised in that step 2
The concentration of middle added sodium hydrate aqueous solution is 10%～30%, consumption be relative fiber raw material 5%～200% (relative to
Fibrous raw material).
The preparation method of a kind of carboxyethylation modified Nano fibrillated fibers the most according to claim 1 element, it is characterised in that step 2
In alkali swollen process the time be 8h～24h.
The preparation method of a kind of carboxyethylation modified Nano fibrillated fibers the most according to claim 1 element, it is characterised in that step 3
The concentration of middle added acrylamide aqueous solution is 5%～50%, and consumption is 5%～200% (relative to fibrous raw material).
The preparation method of a kind of carboxyethylation modified Nano fibrillated fibers the most according to claim 1 element, it is characterised in that step 3
In carboxyethyl modification temperature be 60 DEG C～90 DEG C, the response time be 2h～6h.
The preparation method of a kind of carboxyethylation modified Nano fibrillated fibers the most according to claim 1 element, it is characterised in that step 3
The carboxyethyl content of the carboxyethylation cellulose of preparation is 0.5mmol/g～2.5mmol/g.
The preparation method of a kind of carboxyethylation modified Nano fibrillated fibers the most according to claim 1 element, it is characterised in that step 4
In carboxyethyl cellulose suspension under 1%～4% concentration mechanization process, i.e. obtain stable carboxyethylation nanometer fibrillated fibers
Element.
The preparation method of a kind of carboxyethylation modified Nano fibrillated fibers the most according to claim 1 element, it is characterised in that step 4
In mechanical processing equipment be high pressure homogenizer (including microfluidizer) or fine grinding machine, food processor etc., but not only
It is limited to this.
The preparation method of a kind of carboxyethylation modified Nano fibrillated fibers the most according to claim 1 element, it is characterised in that obtain carboxylic
A diameter of 5nm～100nm of ethylization Nanowire cellulose, length 0.5 μm～10 μm；Carboxyethylation under 0.1% concentration
Nanowire cellulose suspension transmitance under 500nm wavelength is 72%～82%, and the transmitance under 660nm wavelength is
75%～85%.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108530545A (en) * | 2017-03-03 | 2018-09-14 | 重庆市曾东燃纳米科技合伙企业（有限合伙） | A kind of nano-cellulose and preparation method thereof |
| CN109369810A (en) * | 2018-09-18 | 2019-02-22 | 中国制浆造纸研究院有限公司 | Carbamoylethyl fento cellulose and preparation method thereof |
| CN109576810A (en) * | 2018-12-06 | 2019-04-05 | 武汉科丝力纤维制造有限公司 | A kind of preparation method of carboxymethylated cellulosic nanofibrils |
| CN110205856A (en) * | 2018-02-28 | 2019-09-06 | 中国制浆造纸研究院有限公司 | A method of improving fluting medium intensity |
| CN113788900A (en) * | 2021-09-13 | 2021-12-14 | 桂林理工大学 | Modified cellulose nanocrystal with high thermal stability and preparation method thereof |
| CN115637605A (en) * | 2022-10-24 | 2023-01-24 | 金光纸业(中国)投资有限公司 | Lyocell dissolving pulp and preparation method thereof |
| CN116606578A (en) * | 2023-04-14 | 2023-08-18 | 中国皮革制鞋研究院有限公司 | Leather finishing agent and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108530545A (en) * | 2017-03-03 | 2018-09-14 | 重庆市曾东燃纳米科技合伙企业（有限合伙） | A kind of nano-cellulose and preparation method thereof |
| CN110205856A (en) * | 2018-02-28 | 2019-09-06 | 中国制浆造纸研究院有限公司 | A method of improving fluting medium intensity |
| CN110205856B (en) * | 2018-02-28 | 2021-06-15 | 中国制浆造纸研究院有限公司 | Method for improving strength of corrugated base paper |
| CN109369810A (en) * | 2018-09-18 | 2019-02-22 | 中国制浆造纸研究院有限公司 | Carbamoylethyl fento cellulose and preparation method thereof |
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| CN109576810A (en) * | 2018-12-06 | 2019-04-05 | 武汉科丝力纤维制造有限公司 | A kind of preparation method of carboxymethylated cellulosic nanofibrils |
| CN113788900A (en) * | 2021-09-13 | 2021-12-14 | 桂林理工大学 | Modified cellulose nanocrystal with high thermal stability and preparation method thereof |
| CN115637605A (en) * | 2022-10-24 | 2023-01-24 | 金光纸业(中国)投资有限公司 | Lyocell dissolving pulp and preparation method thereof |
| CN115637605B (en) * | 2022-10-24 | 2024-02-13 | 金光纤维(江苏)有限公司 | Lyocell dissolving pulp and preparation method thereof |
| CN116606578A (en) * | 2023-04-14 | 2023-08-18 | 中国皮革制鞋研究院有限公司 | Leather finishing agent and preparation method thereof |
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