CN107446155A - A kind of nano ferriferrous oxide/three-dimensional porous the magnetic composite of salix monogolica/konjaku - Google Patents
A kind of nano ferriferrous oxide/three-dimensional porous the magnetic composite of salix monogolica/konjaku Download PDFInfo
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Abstract
The invention discloses a kind of nano ferriferrous oxide/three-dimensional porous magnetic composite of salix monogolica/konjaku and preparation method thereof, step is as follows：Salix monogolica is removed the peel, crushed, is sieved, is dried, is cooled down, purify after obtain salix cellulose；Salix cellulose is modified using sodium metaperiodate；Use poly-dopamine modified lithium konjaku；By sodium metaperiodate be modified salix cellulose and poly-dopamine modified lithium konjaku it is well mixed after, the trivalent iron salt aqueous solution is slowly dropped into, using obtaining nano ferriferrous oxide/three-dimensional porous magnetic composite of salix monogolica/konjaku after liquid nitrogen, freeze-drying process.The present invention uses konjaku, salix monogolica that magnetic nano ferroferric oxide is carried out into effective self assembly, has potential application value in fields such as sorbing material, biomaterials as raw material.
Description
Technical field
The present invention relates to a kind of nano ferriferrous oxide/three-dimensional porous magnetic composite of salix monogolica/konjaku, belongs to composite
Field.
Background technology
For a long time, cellulose is always weaving, the key industry raw material of papermaking, with its recyclability, biodegradable
Property and cost advantage are increasingly subject to the attention of people, in medicine control, release tech, immobilization technology, biology sensor, membrane material
Material, performance chemicalses and additive etc. show good development prospect.Reduction and oil, natural gas due to arable land etc.
The increasingly depleted of fossil resource, natural fiber, the yield of synthetic fibers will be restricted more and more.And cellulose conduct
A kind of green, environmentally friendly, reproducible resource, obtains a unprecedented opportunity to develop.
Salix monogolica is the desert plant that a kind of only a few can be grown in salt-soda soil.Its sprout is yellow, in leaf is linear or line
Shape lanceolar, branch, which is grown thickly, is not afraid of husky pressure, and well developed root system, rudiment power is strong, is desert-control tree, be mainly distributed on the Inner Mongol,
The ground such as Hebei, Shanxi, Shaanxi, Gansu, Qinghai, Sichuan.Salix monogolica is one of the first choice of " three Norths shelter-forest ", is not only acted as windproof solid
Effect that is husky, conserving water and soil, improving the ecosystem, maintaining ecological balance etc. that also there is unique function.
Salix monogolica in addition to small part is used for pulping and paper-making, fiberboard and composite plate, burn or lose as yule logs by the overwhelming majority
Abandon, cause the huge wasting of resources.The main chemical compositions of salix monogolica mainly have cellulose, hemicellulose, lignin and ash content, fine
The content of element is tieed up in more than 60-70%, is natural reproducible biomass resource, rationally will produce huge warp using salix monogolica resource
Benefit of helping and ecological benefits.At present, most research all concentrates on the cellulose how extracted in salix monogolica.Beijing Forestry University
Department of chemistry engineering Jiang builds new et al. the influence that have studied steam blasting pretreatment to salix monogolica composition and fibre structure performance（Modernization
Work, 2008,28 (2)）.Agricultural University of the Inner Mongol's material science and School of Art and Design Zhang Bin et al. are using salix cellulose as original
Material, have studied the technique that supercritical ultrasonics technology prepares microfibril（Paper and papermaking, 2014,33 (3)）.Agricultural University of the Inner Mongol's material science
With refined et al. main chemical compositions cellulose, the hemicelluloses that salix monogolica material has been isolated using chemical reagent of School of Art and Design Li Ya
Element（Agricultural University of the Inner Mongol's journal, 2014,35 (1)）.Industry light industry textile industry institute of Qiqihar University is permitted phoenix et al. and utilizes peroxidating
Hydrogen method separates salix monogolica and the cellulose in caragana microphylla mixed material（Chemistry of forest product and industry, 2006,26 (2)）.Zhengzhou University's chemical industry
Salix cellulose is extracted with energy institute Huang star et al. use acid catalysis Ethanol Method（Jiangsu's agriculture science, 2014,42 (3)）.
Konjaku glucomannan（Konjac glucomannan, abbreviation KGM）It is after starch and cellulose, one kind is more
Abundant renewable natural polymer child resource, has biodegradable, and its hydrosol has very high viscosity and multifrequency nature
Such as thickening, gel and film forming performance；And a kind of excellent dietary fiber, available for prevention and treatment hypertension, high fat of blood,
The diseases such as cardiovascular disease, it has also become important food additives and healthy food material.In fields such as chemical industry, environmental protection and oil drillings
Also there is important use（Structural chemistry, 2003,06:633-642）.
Using acidified modified, alkali modification, grafting, copolymerization and modification, it is cross-linking modified and etherification modified the methods of can improve KGM's
Performance, for example add alkali deacetylate processing KGM, its strain resistant ability enhancing, mechanical property are improved after processing, therefore natural
KGM and its modified product, turn into one of focus of research（Material Leader, 2009,19:32-36）.Except chemical modification, may be used also
With by being mixed with other suitable biopolymers to improve KGM property（Material Leader, 2009,19:32-36）.Such as
Wuhan University of Technology Fan Li Hong konjaku is made after sodium periodate oxidation oxidation konjaku（OKGM）, utilize its aldehyde radical and hydroxypropyl
Chitosan（HPCS）On amino crosslinking prepare hydrogel, while by graphene oxide（GO）Added as additive in hydrogel
Obtain hydroxypropyl chitosan/oxidized konjaku/graphene oxide hydrogel（Wuhan University Journal (Edition), 2016,04:361-
367）.Guangzhou Business School Huang builds the method for just using physical blending, according to KGM:Silk peptide=1:0,1:2,2:1,0:1 rubs
Your mass ratio prepares blending colloidal sol, and quantitative silk peptide is dissolved in deionized water in the case of stirring, after being completely dissolved, added
Enter quantitative KGM powder, under 45 DEG C of water bath conditions, with 450rmin-11h is stirred, blending colloidal sol is prepared（Concentration is
1.2%）（The biological journal in the torrid zone, 2016,04:472-476）.University Of Agriculture and Forestry In Fujian thanks third clearly according to KGM:Fibroin=1:1、
1:2、1:3 mass ratio is mixed and stirred for being allowed to well mixed, have studied fibroin to konjaku glucomannan（KGM）Structure with
The influence of sol property（Modern food science and technology, 2016,10:125-130+27）.
In addition, also have largely on KGM and hydroxyapatite, montmorillonite, collagen, chitosan, CNT, concave convex rod
The document report of the Material claddings such as soil, starch, soybean protein, graphene（Silicate is circulated a notice of, and 2011,01:162-166+171；In
Jin Chao Institutes Of Technology Of Zhejiang, 2012；Plastics industry, 2010,07:18-20+33；Materials Science and Engineering journal, 2009,06:
870-875+884；Wuhan University Journal (Edition), 2008,02:139-142；Material Leader, 2009,19:32-36；
The preparation method of CN201611262418.5 thermoplasticity konjaku glucomannan nano composite materials；CN201210153668.0 thermoplastics
Property konjaku glucomannan/graphene oxide composite material and preparation method thereof）.But it is multiple to yet there are no salix cellulose/KGM
The open source literature report of condensation material.
The content of the invention
In view of the above problems, the present invention provides a kind of three-dimensional porous magnetic coupling material of nano ferriferrous oxide/salix monogolica/konjaku
Material and preparation method thereof.
The technical scheme is that：
（1）Salix monogolica is removed the peel, crushed, crosses 50-100 mesh sieves, 80-100 DEG C of drying, cooling obtains salix wood powder, then by salix monogolica
Wood powder is added in autoclave, adds absolute ethyl alcohol-acetic acid mixture, bath raio 1:10, wherein the acetic acid addition is
3-5%wt, after being heated to 100-160 DEG C, 1-5h is stirred, is cooled down, filtering, is washed 2-5 times with absolute ethyl alcohol, then use deionized water
Rinse well repeatedly, drying obtains salix cellulose；（2）Salix cellulose in step 1 is scattered in deionized water, bathed
Than 1:50,1-20g/L sodium metaperiodate is then added, lucifuge reacts 30-60min at 50-80 DEG C, repeatedly clear with deionized water
Wash, drying obtains sodium metaperiodate and is modified salix cellulose；（3）Prepare 0.1-10g/L dopamine Tris-HCl buffer solutions, regulation
Konjaku flour is dispersed in 24h in above-mentioned buffer solution, bath raio 1 by pH value at room temperature to 8.5:50, after deionized water is cleaned repeatedly, obtain
To poly-dopamine modified lithium konjaku；（4）Sodium metaperiodate in step 2 is modified the poly-dopamine in salix cellulose and step 3
Modified konjaku is successively scattered in deionized water, bath raio 1:50, it is mixed evenly, 1g/L- is slowly dropped under conditions of 80 DEG C
The 100g/L trivalent iron salt aqueous solution, wherein the mass ratio that the trivalent iron salt is modified salix cellulose with sodium metaperiodate is 1:
5-1:10,80 DEG C of at the uniform velocity stirring reaction 24h, are subsequently poured into mould, are put into 1min in liquid nitrogen, -20 DEG C of refrigerators are placed in after taking-up
Middle pre-freeze 6 hours, freeze 6 hours in -80 DEG C of Thermo ultra low temperature freezers, be then placed in freeze dryer 24 hours, after taking-up
Obtain nano ferriferrous oxide/three-dimensional porous magnetic composite of salix monogolica/konjaku.
Preferably, it is 1 that the sodium metaperiodate, which is modified salix cellulose and the mass ratio of poly-dopamine modified lithium konjaku,:
10-10:1, preferably 1:5-5:1, more preferably 1:2-2:1.
Preferably, the trivalent iron salt is the one or more in iron chloride, ferric sulfate, ferric nitrate.
Compared with prior art, the advantage of the invention is that：
（1）Cellulose fibre is extracted using salix monogolica, raw material is sufficient, cheap, improves the utilization rate of salix monogolica resource, solves
Salix monogolica in addition to small part is used for pulping and paper-making, fiberboard and composite plate, burn or abandon as yule logs, causes by the overwhelming majority
The problem of huge wasting of resources, certain economic benefit and ecological benefits will be produced.（2）Poly-dopamine is a kind of with superpower
The biocompatible materials of Adhesion property, almost can be in any material surface film forming.The forming process of poly-dopamine is simple, reaction
Mild condition, as long as poly- DOPA can be formed in material surface by immersing the material in the Tris-HCl buffer solutions of alkalescence containing dopamine
Amine layer.Sodium metaperiodate is modified the chemical bonds that effect is could be formed between salix cellulose and poly-dopamine modified lithium konjaku.（3）
To be modified salix cellulose and modified konjaku as carrier, nano ferriferrous oxide granule is generated, and at process liquid nitrogen, freeze-drying
The composite obtained after reason has that porosity is high, density is low, intensity is big, high temperature resistant, that specific surface area is big, adsorption capacity is strong etc. is excellent
Point.The composite has certain magnetic, it is possible to achieve effective to recycle.
Embodiment
The invention will be further elucidated with reference to specific embodiments.
Embodiment 1：
（1）Salix monogolica is removed the peel, crushed, crosses 50 mesh sieves, 80 DEG C of drying, cooling obtains salix wood powder, then adds salix wood powder
Into autoclave, absolute ethyl alcohol-acetic acid mixture, bath raio 1 are added:10, wherein the acetic acid addition is 3%wt, add
After hot to 100 DEG C, 1h is stirred, is cooled down, filtering, is washed 2 times with absolute ethyl alcohol, then is rinsed well repeatedly with deionized water, is dried
Obtain salix cellulose；（2）Salix cellulose in step 1 is scattered in deionized water, bath raio 1:50, then add 1g/
L sodium metaperiodate, lucifuge reacts 60min at 50 DEG C, is cleaned repeatedly with deionized water, and drying obtains sodium metaperiodate and is modified salix monogolica
Cellulose；（3）1g/L dopamine Tris-HCl buffer solutions are prepared, konjaku flour is dispersed in by regulation pH value at room temperature to 8.5
State 24h in buffer solution, bath raio 1:50, after deionized water is cleaned repeatedly, obtain poly-dopamine modified lithium konjaku；（4）By in step 2
The poly-dopamine modified lithium konjaku that is modified in salix cellulose and step 3 of sodium metaperiodate be successively scattered in deionized water, wherein
It is 1 that sodium metaperiodate, which is modified salix cellulose and the mass ratio of poly-dopamine modified lithium konjaku,:1, bath raio 1:50, it is mixed evenly,
1g/L ferric chloride in aqueous solution is slowly dropped under conditions of 80 DEG C, wherein the iron chloride is modified salix cellulose with sodium metaperiodate
Mass ratio be 1:5,80 DEG C of at the uniform velocity stirring reaction 24h, are subsequently poured into mould, are put into 1min in liquid nitrogen, -20 are placed in after taking-up
Pre-freeze 6 hours in DEG C refrigerator, freeze 6 hours in -80 DEG C of Thermo ultra low temperature freezers, be then placed in freeze dryer 24 hours,
Nano ferriferrous oxide/three-dimensional porous magnetic composite of salix monogolica/konjaku is obtained after taking-up.
Embodiment 2：
（1）Salix monogolica is removed the peel, crushed, crosses 90 mesh sieves, 80 DEG C of drying, cooling obtains salix wood powder, then adds salix wood powder
Into autoclave, absolute ethyl alcohol-acetic acid mixture, bath raio 1 are added:10, wherein the acetic acid addition is 4%wt, add
After hot to 150 DEG C, 2h is stirred, is cooled down, filtering, is washed 3 times with absolute ethyl alcohol, then is rinsed well repeatedly with deionized water, is dried
Obtain salix cellulose；（2）Salix cellulose in step 1 is scattered in deionized water, bath raio 1:50, then add
10g/L sodium metaperiodate, lucifuge reacts 50min at 70 DEG C, is cleaned repeatedly with deionized water, and drying obtains sodium metaperiodate modification
Salix cellulose；（3）5g/L dopamine Tris-HCl buffer solutions are prepared, regulation pH value at room temperature disperses konjaku flour to 8.5
The 24h in above-mentioned buffer solution, bath raio 1:50, after deionized water is cleaned repeatedly, obtain poly-dopamine modified lithium konjaku；（4）By step
The poly-dopamine modified lithium konjaku that sodium metaperiodate in two is modified in salix cellulose and step 3 is successively scattered in deionized water,
It is 1 that wherein sodium metaperiodate, which is modified salix cellulose and the mass ratio of poly-dopamine modified lithium konjaku,:2, bath raio 1:50, mix equal
It is even, 30g/L ferric sulfate aqueous solution is slowly dropped under conditions of 80 DEG C, wherein the ferric sulfate is modified salix monogolica with sodium metaperiodate
The mass ratio of cellulose is 1:7,80 DEG C of at the uniform velocity stirring reaction 24h, are subsequently poured into mould, 1min in liquid nitrogen are put into, after taking-up
Pre-freeze 6 hours in -20 DEG C of refrigerators are placed in, freezes 6 hours, is then placed in freeze dryer in -80 DEG C of Thermo ultra low temperature freezers
24 hours, nano ferriferrous oxide/three-dimensional porous magnetic composite of salix monogolica/konjaku is obtained after taking-up.
Embodiment 3：
（1）Salix monogolica is removed the peel, crushed, crosses 100 mesh sieves, 100 DEG C of drying, cooling obtains salix wood powder, then adds salix wood powder
It is added in autoclave, adds absolute ethyl alcohol-acetic acid mixture, bath raio 1:10, wherein the acetic acid addition is 5%wt,
After being heated to 160 DEG C, 5h is stirred, is cooled down, filtering, is washed 5 times with absolute ethyl alcohol, then is rinsed well repeatedly with deionized water, is dried
It is dry to obtain salix cellulose；（2）Salix cellulose in step 1 is scattered in deionized water, bath raio 1:50, then add
20g/L sodium metaperiodate, lucifuge reacts 30min at 80 DEG C, is cleaned repeatedly with deionized water, and drying obtains sodium metaperiodate modification
Salix cellulose；（3）Prepare 10g/L dopamine Tris-HCl buffer solutions, regulation pH value to 8.5, at room temperature by konjaku flour point
It is dispersed in 24h in above-mentioned buffer solution, bath raio 1:50, after deionized water is cleaned repeatedly, obtain poly-dopamine modified lithium konjaku；（4）Will step
The poly-dopamine modified lithium konjaku that sodium metaperiodate in rapid two is modified in salix cellulose and step 3 is successively scattered in deionized water
In, it is 2 that wherein sodium metaperiodate, which is modified salix cellulose and the mass ratio of poly-dopamine modified lithium konjaku,:1, bath raio 1:50, mixing is stirred
The iron nitrate aqueous solution that 100g/L uniformly, is slowly dropped under conditions of 80 DEG C is mixed, wherein the ferric nitrate is modified with sodium metaperiodate
The mass ratio of salix cellulose is 1:10,80 DEG C of at the uniform velocity stirring reaction 24h, are subsequently poured into mould, are put into 1min in liquid nitrogen, take
Pre-freeze 6 hours in -20 DEG C of refrigerators are placed in after going out, are freezed 6 hours in -80 DEG C of Thermo ultra low temperature freezers, are then placed in lyophilized
24 hours in machine, nano ferriferrous oxide/three-dimensional porous magnetic composite of salix monogolica/konjaku is obtained after taking-up.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention.For those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms.Here all embodiments can not be exhaustive.It is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is amplified out still in protection scope of the present invention.
Claims (5)
- A kind of 1. preparation method of nano ferriferrous oxide/three-dimensional porous magnetic composite of salix monogolica/konjaku, it is characterised in that：Step 1：Salix monogolica is removed the peel, crushed, crosses 50-100 mesh sieves, 80-100 DEG C of drying, cooling obtains salix wood powder, then will Salix wood powder is added in autoclave, adds absolute ethyl alcohol-acetic acid mixture, bath raio 1:10, wherein the acetic acid adds Measure as 3-5%wt, after being heated to 100-160 DEG C, stir 1-5h, cool down, filtering, washed 2-5 times with absolute ethyl alcohol, then spend from Sub- water is rinsed well repeatedly, and drying obtains salix cellulose；Step 2：Salix cellulose in step 1 is scattered in deionized water, bath raio 1:50, then add 1-20g/L's Sodium metaperiodate, lucifuge reacts 30-60min at 50-80 DEG C, is cleaned repeatedly with deionized water, and drying obtains sodium metaperiodate modification Salix cellulose；Step 3：Prepare 0.1-10g/L dopamine Tris-HCl buffer solutions, regulation pH value to 8.5, at room temperature by konjaku flour point It is dispersed in 24h in above-mentioned buffer solution, bath raio 1:50, after deionized water is cleaned repeatedly, obtain poly-dopamine modified lithium konjaku；Step 4：Poly-dopamine modified lithium konjaku priority sodium metaperiodate in step 2 being modified in salix cellulose and step 3 It is scattered in deionized water, bath raio 1:50, it is mixed evenly, 1g/L-100g/L trivalent is slowly dropped under conditions of 80 DEG C Molysite aqueous solution, wherein the mass ratio that the trivalent iron salt is modified salix cellulose with sodium metaperiodate is 1:5-1:10,80 DEG C even Fast stirring reaction 24h, is subsequently poured into mould, is put into 1min in liquid nitrogen, and pre-freeze 6 hours in -20 DEG C of refrigerators are placed in after taking-up, - Freeze 6 hours, be then placed in freeze dryer 24 hours in 80 DEG C of Thermo ultra low temperature freezers, nanometer four is obtained after taking-up and is aoxidized Three-iron/three-dimensional porous the magnetic composite of salix monogolica/konjaku.
- A kind of 2. system of nano ferriferrous oxide/three-dimensional porous magnetic composite of salix monogolica/konjaku according to claim 1 Preparation Method, it is characterised in that it is 1 that the sodium metaperiodate, which is modified salix cellulose and the mass ratio of poly-dopamine modified lithium konjaku,:10- 10:1。
- A kind of 3. system of nano ferriferrous oxide/three-dimensional porous magnetic composite of salix monogolica/konjaku according to claim 1 Preparation Method, it is characterised in that the sodium metaperiodate is modified salix cellulose and the mass ratio of poly-dopamine modified lithium konjaku is preferably 1:5-5:1, more preferably 1:2-2:1.
- A kind of 4. system of nano ferriferrous oxide/three-dimensional porous magnetic composite of salix monogolica/konjaku according to claim 1 Preparation Method, it is characterised in that the trivalent iron salt is the one or more in iron chloride, ferric sulfate, ferric nitrate.
- A kind of 5. three-dimensional porous magnetic coupling material of nano ferriferrous oxide/salix monogolica/konjaku obtained by claim 1 preparation method Material.
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| CN201710836597.7A CN107446155A (en) | 2017-09-17 | 2017-09-17 | A kind of nano ferriferrous oxide/three-dimensional porous the magnetic composite of salix monogolica/konjaku |
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| CN201710836597.7A CN107446155A (en) | 2017-09-17 | 2017-09-17 | A kind of nano ferriferrous oxide/three-dimensional porous the magnetic composite of salix monogolica/konjaku |
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| CN107446155A true CN107446155A (en) | 2017-12-08 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108214813A (en) * | 2017-12-23 | 2018-06-29 | 仇颖超 | A kind of preparation method of recyclable absorbent-type magnetic timber |
| CN111759011A (en) * | 2020-07-11 | 2020-10-13 | 罗金火 | Porous body for liquid storage |
| CN111808581A (en) * | 2020-07-22 | 2020-10-23 | 西南石油大学 | Chitosan graphene oxide nano hydrogel plugging agent and water-based drilling fluid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104233495A (en) * | 2014-10-15 | 2014-12-24 | 钱景 | Salix mongolica regenerated cellulose and preparation method thereof |
| CN104479174A (en) * | 2014-12-14 | 2015-04-01 | 苏州大学 | Cellulose-based magnetic aerogel material and preparation method thereof |
| CN105344331A (en) * | 2015-10-15 | 2016-02-24 | 顺德职业技术学院 | Spherical heavy metal capture and adsorption material and preparation method thereof |
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2017
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104233495A (en) * | 2014-10-15 | 2014-12-24 | 钱景 | Salix mongolica regenerated cellulose and preparation method thereof |
| CN104479174A (en) * | 2014-12-14 | 2015-04-01 | 苏州大学 | Cellulose-based magnetic aerogel material and preparation method thereof |
| CN105344331A (en) * | 2015-10-15 | 2016-02-24 | 顺德职业技术学院 | Spherical heavy metal capture and adsorption material and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108214813A (en) * | 2017-12-23 | 2018-06-29 | 仇颖超 | A kind of preparation method of recyclable absorbent-type magnetic timber |
| CN111759011A (en) * | 2020-07-11 | 2020-10-13 | 罗金火 | Porous body for liquid storage |
| CN111808581A (en) * | 2020-07-22 | 2020-10-23 | 西南石油大学 | Chitosan graphene oxide nano hydrogel plugging agent and water-based drilling fluid |
| CN111808581B (en) * | 2020-07-22 | 2022-04-19 | 西南石油大学 | Chitosan graphene oxide nano hydrogel plugging agent and water-based drilling fluid |
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