CN107556518A - Graphene oxide salix monogolica konjaku cyclodextrin composite and preparation method - Google Patents
Graphene oxide salix monogolica konjaku cyclodextrin composite and preparation method Download PDFInfo
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- CN107556518A CN107556518A CN201710836589.2A CN201710836589A CN107556518A CN 107556518 A CN107556518 A CN 107556518A CN 201710836589 A CN201710836589 A CN 201710836589A CN 107556518 A CN107556518 A CN 107556518A
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Abstract
The invention discloses graphene oxide salix monogolica konjaku cyclodextrin composite and preparation method, by weight percentage, 40 50% salix monogolica beta cyclodextrin composites and 40 50% PAMAM modified konjakus, 1 20% graphene oxide, 1 5% pore-foaming agent are successively scattered in deionized water, bath raio 1:50, after ultrasonic mixing is uniform, at the uniform velocity stirring reaction 24h under normal temperature；It is subsequently poured into mould, is put into 1min in liquid nitrogen, pre-freeze 6h in 20 DEG C of refrigerators is placed in after taking-up, 6h is freezed in 80 DEG C of Thermo ultra low temperature freezers, is then placed in 48h in freeze dryer and obtains graphene oxide salix monogolica konjaku cyclodextrin composite.The present invention uses graphene oxide, konjaku, salix monogolica, beta cyclodextrin to have the advantages that raw material is sufficient, cheap as raw material, have important application value in fields such as sorbing material, biomaterials.
Description
Technical field
The present invention relates to a kind of graphene oxide-salix monogolica-konjaku-cyclodextrin composite, belongs to field of compound material.
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, the yield of synthetic fibers will be restricted more and more.And a kind of green of cellulose conduct,
Environmentally friendly, reproducible resource, obtain 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）.
, can also be by being mixed with other suitable biopolymers to improve KGM property except chemical modification（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 and 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 molal weight is molten by quantitative silk peptide in the case of stirring than preparing blending colloidal sol
In deionized water, after being completely dissolved, add quantitative KGM powder, under 45 DEG C of water bath conditions, with 450rmin-1Stirring
1h, 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 is thanked
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 silk egg
In vain to konjaku glucomannan（KGM）The influence of structure and 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 there is not salix cellulose/KGM/ also at present
The open source literature report of beta-schardinger dextrin composite.
The content of the invention
In view of the above problems, the present invention provides graphene oxide-salix monogolica-konjaku-cyclodextrin composite and preparation method.
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, beta-schardinger dextrin is then added, after being mixed evenly, adds 1-100g/L sodium metaperiodate, the lucifuge at 50-80 DEG C
60-300min is reacted, is cleaned repeatedly with deionized water, drying obtains salix monogolica-beta-schardinger dextrin composite.（3）By evil spirit under normal temperature
Taro powder is scattered in deionized water, bath raio 1:50, glutaraldehyde is added, the volume ratio of wherein glutaraldehyde and konjaku amidin is 1:
10, be mixed evenly, be then slowly added into the 1-100g/L polyamide-amide PAMAM aqueous solution, wherein the PAMAM aqueous solution with
The volume ratio of konjaku amidin is 1:1-1:10, after reacting 24h, washed with distilled water and ethanol, obtained after drying repeatedly
PAMAM modified konjakus.（4）By weight percentage, 40-50% salix monogolicas-beta-schardinger dextrin composite and 40-50% PAMAM are changed
Property konjaku, 1-20% graphene oxides, 1-5% pore-foaming agents successively be scattered in deionized water, bath raio 1:50, ultrasonic mixing is uniform
Afterwards, at the uniform velocity stirring reaction 24h under normal temperature；It is subsequently poured into mould, is put into 1min in liquid nitrogen, is placed in after taking-up in -20 DEG C of refrigerators
Pre-freeze 6h, 6h is freezed in -80 DEG C of Thermo ultra low temperature freezers, 48h in freeze dryer is then placed in and obtains graphene oxide-sand
Willow-konjaku-cyclodextrin composite.
Preferably, beta-schardinger dextrin described in step 2 and the mass ratio of salix cellulose are 1:10-10:1, preferably
For 1:5-5:1, more preferably 1:2-2:1.
Preferably, the pore-foaming agent is lauryl sodium sulfate, cetyl trimethylammonium bromide, polyethylene glycol
In one or more.
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）Sodium metaperiodate is modified to a certain extent
The crystal region of salix cellulose and beta-schardinger dextrin is destroyed, so as to be advantageous in salix cellulose and beta-schardinger dextrin macromolecular chain
Upper grafting functional group.PAMAM is polyamidoamine dendrimer, and surface is rich in amino, imido grpup.Thus salix monogolica-β-
It can be produced between cyclodextrin composite, PAMAM modified konjakus and graphene oxide by chemical bond, hydrogen bond, Van der Waals force
Firm to combine, the graphene oxide-salix monogolica-konjaku-cyclodextrin composite being prepared has that density is low, intensity is big, resistance to
The advantages that high temperature, specific surface area are big, adsorption capacity is strong.
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 β-
The mass ratio of cyclodextrin, wherein beta-schardinger dextrin and salix cellulose is 1:1, after being mixed evenly, add 20g/L periodic acid
Sodium, lucifuge reacts 300min at 50 DEG C, is cleaned repeatedly with deionized water, and drying obtains salix monogolica-beta-schardinger dextrin composite；
（3）Konjaku flour is scattered in deionized water under normal temperature, bath raio 1:50, glutaraldehyde is added, wherein glutaraldehyde and konjaku flour is water-soluble
The volume ratio of liquid is 1:10, it is mixed evenly, is then slowly added into the 50g/L polyamide-amide PAMAM aqueous solution, wherein
The volume ratio of the PAMAM aqueous solution and konjaku amidin is 1:1, after reacting 24h, washed, dried repeatedly with distilled water and ethanol
After obtain PAMAM modified konjakus；（4）By weight percentage, 40% salix monogolica-beta-schardinger dextrin composite and 40% PAMAM are changed
Property konjaku, 15% graphene oxide, 5% lauryl sodium sulfate successively be scattered in deionized water, bath raio 1:50, ultrasonic mixing is equal
After even, at the uniform velocity stirring reaction 24h under normal temperature；It is subsequently poured into mould, is put into 1min in liquid nitrogen, -20 DEG C of refrigerators are placed in after taking-up
Middle pre-freeze 6h, 6h is freezed in -80 DEG C of Thermo ultra low temperature freezers, 48h in freeze dryer is then placed in and obtains graphene oxide-sand
Willow-konjaku-cyclodextrin composite.
Embodiment 2：
（1）Salix monogolica is removed the peel, crushed, crosses 80 mesh sieves, 90 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 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 β-
The mass ratio of cyclodextrin, wherein beta-schardinger dextrin and salix cellulose is 1:2, after being mixed evenly, add 50g/L periodic acid
Sodium, lucifuge reacts 100min at 80 DEG C, is cleaned repeatedly with deionized water, and drying obtains salix monogolica-beta-schardinger dextrin composite；
（3）Konjaku flour is scattered in deionized water under normal temperature, bath raio 1:50, glutaraldehyde is added, wherein glutaraldehyde and konjaku flour is water-soluble
The volume ratio of liquid is 1:10, it is mixed evenly, is then slowly added into the 10g/L polyamide-amide PAMAM aqueous solution, wherein
The volume ratio of the PAMAM aqueous solution and konjaku amidin is 1:6, after reacting 24h, washed, dried repeatedly with distilled water and ethanol
After obtain PAMAM modified konjakus；（4）By weight percentage, 40% salix monogolica-beta-schardinger dextrin composite and 40% PAMAM are changed
Property konjaku, 19% graphene oxide, 1% cetyl trimethylammonium bromide successively be scattered in deionized water, bath raio 1:50, ultrasound
After well mixed, at the uniform velocity stirring reaction 24h under normal temperature；It is subsequently poured into mould, is put into 1min in liquid nitrogen, -20 are placed in after taking-up
Pre-freeze 6h in DEG C refrigerator, 6h is freezed in -80 DEG C of Thermo ultra low temperature freezers, 48h in freeze dryer is then placed in and obtains aoxidizing stone
Black alkene-salix monogolica-konjaku-cyclodextrin composite.
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, 4h 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
The mass ratio of beta-schardinger dextrin, wherein beta-schardinger dextrin and salix cellulose is 2:1, after being mixed evenly, add 100g/L height
Sodium iodate, lucifuge reacts 60min at 80 DEG C, is cleaned repeatedly with deionized water, and drying obtains salix monogolica-beta-schardinger dextrin composite wood
Material；（3）Konjaku flour is scattered in deionized water under normal temperature, bath raio 1:50, add glutaraldehyde, wherein glutaraldehyde and konjaku flour water
The volume ratio of solution is 1:10, it is mixed evenly, is then slowly added into the 100g/L polyamide-amide PAMAM aqueous solution, wherein
The volume ratio of the PAMAM aqueous solution and konjaku amidin is 1:10, after reacting 24h, washed, dried repeatedly with distilled water and ethanol
After obtain PAMAM modified konjakus；（4）By weight percentage, 44% salix monogolica-beta-schardinger dextrin composite and 46% PAMAM are changed
Property konjaku, 8% graphene oxide, 2% polyethylene glycol successively be scattered in deionized water, bath raio 1:50, after ultrasonic mixing is uniform, often
At the uniform velocity stirring reaction 24h under temperature；It is subsequently poured into mould, is put into 1min in liquid nitrogen, pre-freeze in -20 DEG C of refrigerators is placed in after taking-up
6h, 6h is freezed in -80 DEG C of Thermo ultra low temperature freezers, 48h in freeze dryer is then placed in and obtains graphene oxide-salix monogolica-evil spirit
Taro-cyclodextrin composite.
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 graphene oxide-salix monogolica-konjaku-cyclodextrin composite, 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, beta-schardinger dextrin is then added, After being mixed evenly, 1-100g/L sodium metaperiodate is added, lucifuge reacts 60-300min at 50-80 DEG C, uses deionized water Clean repeatedly, drying obtains salix monogolica-beta-schardinger dextrin composite；Step 3：Konjaku flour is scattered in deionized water under normal temperature, bath raio 1:50, add glutaraldehyde, wherein glutaraldehyde and evil spirit The volume ratio of taro amidin is 1:10, it is mixed evenly, is then slowly added into 1-100g/L polyamide-amide PAMAM water The volume ratio of solution, wherein the PAMAM aqueous solution and konjaku amidin is 1:1-1:10, after reacting 24h, with distilled water and ethanol Wash repeatedly, obtain PAMAM modified konjakus after drying；Step 4：By weight percentage, 40-50% salix monogolicas-beta-schardinger dextrin composite and 40-50% PAMAM are modified evil spirit Taro, 1-20% graphene oxides, 1-5% pore-foaming agents are successively scattered in deionized water, bath raio 1:50, after ultrasonic mixing is uniform, often At the uniform velocity stirring reaction 24h under temperature；It is subsequently poured into mould, is put into 1min in liquid nitrogen, pre-freeze in -20 DEG C of refrigerators is placed in after taking-up 6h, 6h is freezed in -80 DEG C of Thermo ultra low temperature freezers, 48h in freeze dryer is then placed in and obtains graphene oxide-salix monogolica-evil spirit Taro-cyclodextrin composite.
- 2. a kind of preparation method of graphene oxide-salix monogolica-konjaku-cyclodextrin composite according to claim 1, its It is characterised by, the mass ratio of beta-schardinger dextrin described in step 2 and salix cellulose is 1:10-10:1.
- 3. a kind of preparation method of graphene oxide-salix monogolica-konjaku-cyclodextrin composite according to claim 1, its It is characterised by, the mass ratio of beta-schardinger dextrin described in step 2 and salix cellulose is preferably 1:5-5:1, more preferably 1: 2-2:1。
- 4. a kind of preparation method of graphene oxide-salix monogolica-konjaku-cyclodextrin composite according to claim 1, its It is characterised by, the pore-foaming agent is lauryl sodium sulfate, cetyl trimethylammonium bromide, one kind in polyethylene glycol or more Kind.
- A kind of 5. graphene oxide-salix monogolica-konjaku-cyclodextrin composite obtained by claim 1 preparation method.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108744591A (en) * | 2018-04-20 | 2018-11-06 | 中国石油化工股份有限公司 | The extracting process of chromocor compound |
| 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 |
| CN113024859A (en) * | 2021-03-02 | 2021-06-25 | 林香春 | Edible antibacterial medicine packaging film and preparation method thereof |
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| CN103480348A (en) * | 2013-10-16 | 2014-01-01 | 苏州大学 | Preparation method of modified cellulose adsorbents |
| CN104264259A (en) * | 2014-10-15 | 2015-01-07 | 钱景 | Graphene and salix psammophila regenerated cellulose blended fiber 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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| CN103480348A (en) * | 2013-10-16 | 2014-01-01 | 苏州大学 | Preparation method of modified cellulose adsorbents |
| CN104264259A (en) * | 2014-10-15 | 2015-01-07 | 钱景 | Graphene and salix psammophila regenerated cellulose blended fiber 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 (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108744591A (en) * | 2018-04-20 | 2018-11-06 | 中国石油化工股份有限公司 | The extracting process of chromocor compound |
| 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 |
| CN113024859A (en) * | 2021-03-02 | 2021-06-25 | 林香春 | Edible antibacterial medicine packaging film and preparation method thereof |
| CN114805948A (en) * | 2021-03-02 | 2022-07-29 | 林香春 | Edible antibacterial medicine packaging film |
| CN113024859B (en) * | 2021-03-02 | 2022-12-06 | 苏州鱼得水电气科技有限公司 | Edible antibacterial medicine packaging film and preparation method thereof |
| CN114805948B (en) * | 2021-03-02 | 2023-06-23 | 马丁医用包装(珠海)有限公司 | Edible antibacterial medicine packaging film |
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