CN107159163A - A kind of preparation method of the cellulose base composite aerogel of high absorption property - Google Patents

A kind of preparation method of the cellulose base composite aerogel of high absorption property Download PDF

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Publication number
CN107159163A
CN107159163A CN201710429529.9A CN201710429529A CN107159163A CN 107159163 A CN107159163 A CN 107159163A CN 201710429529 A CN201710429529 A CN 201710429529A CN 107159163 A CN107159163 A CN 107159163A
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CN
China
Prior art keywords
dopamine
cellulose
composite aerogel
poly
base composite
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Pending
Application number
CN201710429529.9A
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Chinese (zh)
Inventor
王勇
韦枭
杨静晖
黄婷
张楠
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Southwest Jiaotong University
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Southwest Jiaotong University
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Priority to CN201710429529.9A priority Critical patent/CN107159163A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26Synthetic macromolecular compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28047Gels
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/285Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

The invention discloses a kind of preparation method of the cellulose base composite aerogel with high absorption property, dopamine powder is dissolved in 50% 80% lithium bromide water solution, microcrystalline cellulose powder is added, dopamine is 1 with microcrystalline cellulose weight ratio:0.75‑1:1.5, it is placed in 120 DEG C of oil baths, microcrystalline cellulose dissolves under 50 100r/min stirring conditions, dissolution time is 40min or so, meanwhile, dopamine auto polymerization forms poly-dopamine;Solution is placed in room temperature freeze-drying after slowly cooling and forms poly-dopamine/cellulose base composite aerogel.The composite aerogel of the present invention has excellent absorption property to positive dyestuff methylene blue, and its technique is relatively simple.

Description

A kind of preparation method of the cellulose base composite aerogel of high absorption property
Technical field
The present invention relates to field of environmental improvement, more specifically, it is related to a kind of preparation method of the adsorbent of high absorption property.
Background technology
In recent decades, the quickening of process of industrialization and the sharp increase of population cause serious environmental pollution.Its reclaimed water is dirty Dye is particularly acute, substantial amounts of toxic heavy metal ion, inorganic anion, organic micro-pollutantses, such as dyestuff, phenols, agricultural chemicals, humic Sour organic compound, detergent and other persistence organic pollutants, in wide coverage all over the world in recent decades.This A little toxic pollutants are discharged into water body, greatly affected the ecological balance, harmful effect is caused to animals and plants.In addition these are dirty Thing not only chemically-resistant and biodegradation is contaminated, and has very big environment mobility, is had simultaneously for the biological concentration in food chain Very strong trend.Therefore, we are necessary to be handled these sewage before natural water is discharged into.
Existing a variety for the treatment of technologies can reduce the pollutant concentration in waste water at present, including chemistry redox, UF membrane, Extraction, ion exchange and electrodialysis etc., the validity and cost of these methods are variant.Compare at several different physical chemistry The method for managing sewage, in numerous treatment technologies, charcoal absorption is because its removal efficiency is high, produced without harmful side product, quilt It is considered as one of optimal alternative solution of removal water pollutant.But the production of activated carbon is relative complex, be directed to carbonization and Activation stage, although its water treatment efficiency is favourable, the production cost of great number cause activated carbon can not as adsorbent poor or Developing country is used for large-scale water process, therefore, and inexpensive, efficient adsorbent turns into the emphasis that people study.
The content of the invention
, should it is an object of the invention to provide a kind of preparation method of the cellulose base composite aerogel with high absorption property Composite aerogel prepared by method has excellent absorption property to positive dyestuff methylene blue, and its technique is relatively simple.
A kind of preparation method of the cellulose base composite aerogel of high absorption property of the present invention, has main steps that:
A. the lithium bromide water solution by weight for 60% is prepared;
B. dopamine powder is added in lithium bromide water solution, is dissolved under conditions of stirring, add microcrystalline cellulose Powder, wherein, dopamine is 1 with microcrystalline cellulose weight ratio:0.75-1:1.5;
C. it is placed in 120 DEG C of oil baths, microcrystalline cellulose dissolves under 50-100r/min stirring conditions, and dissolution time is 40min Left and right, meanwhile, dopamine auto polymerization forms poly-dopamine;
D. until cellulose is completely dissolved, solution is placed in room temperature and is cooled slowly until to form poly-dopamine/cellulose Gel;
E. deionized water is added into poly-dopamine/cellulose gel, constantly replaces deionized water, until removing bromine completely Change lithium, poly-dopamine/cellulose base composite aerogel is produced by freeze-drying.
In a kind of preparation method of the cellulose base composite aerogel of high absorption property of the present invention, described microcrystalline cellulose Element is in granular form, and its particle diameter is about 25 μm.
In a kind of preparation method of the cellulose base composite aerogel of high absorption property of the present invention, described lithium bromide water Solution is 60%.
Compared with prior art, the beneficial effects of the invention are as follows:
1) present invention is used makes aeroge by cellulose, significantly increases the porosity and ratio of cellulose aerogels Surface area, and preparation method is simple, while polymerizeing dopamine in aeroge situ so that poly-dopamine is uniformly dispersed in Inside cellulose aerogels, adsorption capacity of the cellulose aerogels to methylene blue is greatly improved.With pure cellulose airsetting Glue is compared, and poly-dopamine/cellulose base composite aerogel improves 47.29% to the adsorption efficiency of methylene blue.
2) present invention is used as matrix using microcrystalline cellulose.Cellulose is natural polymer most ancient on the earth and most rich Rich renewable resource, it is mainly derived from trees, bamboo, cotton, reed and other higher plants.Produced about on the annual earth 200000000000 tons of plant celluloses, are inexhaustible, the nexhaustible renewable resources of nature.Therefore, for native cellulose The high value added utilization of this non-fossil renewable natural resources, and high performance-price ratio " green " sorbing material industry and technology Demand, cellulose base sorbing material of the research and development with independent intellectual property right, for extension China fiber-composite industrial chain, Strategic high-tech demand and international competitiveness are met, it is significant.
3) present invention poly-dopamine used is modified to cellulose aerogels.The molecular structure of poly-dopamine is similar to and made a gift of The structure of shellfish attachment proteins, has the advantages that the latter's adhesiveness, can easily stick to almost all kinds of surface, bag Include from organic to inorganic, or even super hydrophobic surface.In addition, the auto polymerization conditioned response of dopamine is gentle, it is not necessary to by The reaction condition of any complicated instrument or harshness, poly-dopamine is introduced into cellulose aerogels by the present invention is used for dyestuff suction It is attached, play the absorption property of poly-dopamine.
Further, poly-dopamine of the invention is a kind of extremely strong polymer of adhesiveness, is introduced into cellulose aerogels Inside greatly improves adsorption capacity of the composite aerogel to methylene blue.
Further, the concrete operations in a certain amount of dopamine powder addition LiBr aqueous solution are by the present invention:Temperature For 20-25 DEG C, mixing time is 10min or so, and with 50-100r/min stirring.So ensure that dopamine is completely dissolved.
Further, the present invention by cellulose powder add LiBr the aqueous solution in concrete operations be:Temperature is 120 DEG C, dissolution time is 40min, and with 50-100r/min stirring.So ensure that cellulose is completely dissolved.
Embodiment
The present invention is described in further details with reference to embodiment.
Embodiment 1
60wt% lithium bromide water solution (LiBr) 5ml is prepared, 50mg dopamine powder is added into the water-soluble of lithium bromide In liquid,:Temperature is 20-25 DEG C, and mixing time is 10min or so, and with 50-100r/min stirring.So ensure DOPA Amine is completely dissolved.Then 75mg microcrystalline cellulose powder is added, is placed in 120 DEG C of oil baths and dissolves under agitation, dissolving Time is 40min, and with 50-100r/min stirring.Auto polymerization forms poly-dopamine to dopamine at high temperature simultaneously;Until Cellulose is completely dissolved, and poly-dopamine/cellulose solution is placed in room temperature and is cooled slowly until to form gel, then to poly- many Deionized water is added in bar amine/cellulose gel, constantly deionized water is exchanged until removing lithium bromide, the poly- DOPA of gained completely Amine/cellulose aquagel produces poly-dopamine/cellulose base composite aerogel by freeze-drying.
Microcrystalline cellulose wherein used in the present invention is in granular form, and its particle diameter is about 25 μm.
Embodiment 2
60wt% lithium bromide water solution (LiBr) 5ml is prepared, 75mg dopamine powder is added into the water-soluble of lithium bromide In liquid, by DOPA amine solvent under conditions of stirring, 75mg microcrystalline cellulose powder is then added, is placed under agitation Dissolved in 120 DEG C of oil baths, while auto polymerization forms poly-dopamine to dopamine at high temperature;Until cellulose is completely dissolved, will be poly- Dopamine/cellulose solution, which is placed in room temperature, to be cooled slowly until to form gel, is then added into poly-dopamine/cellulose gel Enter deionized water, constantly exchange deionized water until removing LiBr completely, gained poly-dopamine/cellulose aquagel passes through freezing It is drying to obtain poly-dopamine/cellulose base composite aerogel.
Embodiment 3
60wt% lithium bromide water solution (LiBr) 5ml is prepared, 100mg dopamine powder is added to the LiBr aqueous solution In, by DOPA amine solvent under conditions of stirring, 75mg microcrystalline cellulose powder is then added, is placed under agitation Dissolved in 120 DEG C of oil baths, while auto polymerization forms poly-dopamine to dopamine at high temperature;Until cellulose is completely dissolved, will be poly- Dopamine/cellulose solution, which is placed in room temperature, to be cooled slowly until to form gel, is then added into poly-dopamine/cellulose gel Enter deionized water, constantly exchange deionized water until removing LiBr completely, gained poly-dopamine/cellulose aquagel passes through freezing It is drying to obtain poly-dopamine/cellulose base composite aerogel.

Claims (3)

1. a kind of preparation method of the cellulose base composite aerogel of high absorption property, has main steps that:
A. the lithium bromide water solution by weight for 50%-80% is prepared;
B. dopamine powder is added in lithium bromide water solution, is dissolved under conditions of stirring, add microcrystalline cellulose powder, Wherein, dopamine and microcrystalline cellulose weight ratio are 1:0.75-1:1.5;
C. it is placed in 120 DEG C of oil baths, microcrystalline cellulose dissolves under 50-100r/min stirring conditions, dissolution time is 40min left The right side, meanwhile, dopamine auto polymerization forms poly-dopamine;
D. until cellulose is completely dissolved, solution is placed in room temperature and is cooled slowly until to form poly-dopamine/cellulose gel;
E. deionized water is added into poly-dopamine/cellulose gel, constantly replaces deionized water, until removing bromination completely Lithium, poly-dopamine/cellulose base composite aerogel is produced by freeze-drying.
2. a kind of preparation method of the cellulose base composite aerogel of high absorption property according to claim 1, its feature It is, described microcrystalline cellulose is in granular form, its particle diameter is about 25 μm.
3. a kind of preparation method of the cellulose base composite aerogel of high absorption property according to claim 1, its feature It is, wherein, lithium bromide water solution is 60%.
CN201710429529.9A 2017-06-08 2017-06-08 A kind of preparation method of the cellulose base composite aerogel of high absorption property Pending CN107159163A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108752606A (en) * 2018-06-26 2018-11-06 西南交通大学 Cellulose composite hydrogel for Dye Adsorption and preparation method thereof and aeroge and preparation method thereof
CN108774343A (en) * 2018-06-26 2018-11-09 西南交通大学 Composite aerogel and preparation method thereof and composite hydrogel and preparation method thereof
CN108839408A (en) * 2018-05-18 2018-11-20 浙江鹏远新材料股份有限公司 A kind of corrosion resistant heat-insulating heat-preserving material and preparation method thereof
CN109174020A (en) * 2018-08-07 2019-01-11 济南大学 A kind of preparation method of poly-dopamine modified lithium cellulose aerogels coating solid phase micro-extraction fiber
CN109225160A (en) * 2018-10-29 2019-01-18 西南交通大学 A kind of cellulose base porous aerogel and preparation method thereof with Photocatalytic activity
CN111849019A (en) * 2020-07-31 2020-10-30 河海大学 Preparation method of cellulose composite aerogel
CN112831085A (en) * 2020-12-30 2021-05-25 浙江海洋大学 Preparation of oil-water separation cellulose aerogel
CN118440391A (en) * 2024-04-25 2024-08-06 南京林业大学 Polydopamine-nanocellulose composite aerogel material, and preparation method and application thereof

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CN105289527A (en) * 2015-12-03 2016-02-03 南京林业大学 Preparation method of cellulose ester aerogel material for adsorbing organic matters in wastewater
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CN106076283A (en) * 2016-06-11 2016-11-09 华南理工大学 A kind of nano-cellulose/poly-dopamine hydrogel adsorbent and preparation method and application

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CN105289527A (en) * 2015-12-03 2016-02-03 南京林业大学 Preparation method of cellulose ester aerogel material for adsorbing organic matters in wastewater
CN106076283A (en) * 2016-06-11 2016-11-09 华南理工大学 A kind of nano-cellulose/poly-dopamine hydrogel adsorbent and preparation method and application

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108839408A (en) * 2018-05-18 2018-11-20 浙江鹏远新材料股份有限公司 A kind of corrosion resistant heat-insulating heat-preserving material and preparation method thereof
CN108752606A (en) * 2018-06-26 2018-11-06 西南交通大学 Cellulose composite hydrogel for Dye Adsorption and preparation method thereof and aeroge and preparation method thereof
CN108774343A (en) * 2018-06-26 2018-11-09 西南交通大学 Composite aerogel and preparation method thereof and composite hydrogel and preparation method thereof
CN109174020A (en) * 2018-08-07 2019-01-11 济南大学 A kind of preparation method of poly-dopamine modified lithium cellulose aerogels coating solid phase micro-extraction fiber
CN109174020B (en) * 2018-08-07 2021-07-27 济南大学 Preparation method of polydopamine modified cellulose aerogel coating solid-phase microextraction fiber
CN109225160A (en) * 2018-10-29 2019-01-18 西南交通大学 A kind of cellulose base porous aerogel and preparation method thereof with Photocatalytic activity
CN111849019A (en) * 2020-07-31 2020-10-30 河海大学 Preparation method of cellulose composite aerogel
CN112831085A (en) * 2020-12-30 2021-05-25 浙江海洋大学 Preparation of oil-water separation cellulose aerogel
CN118440391A (en) * 2024-04-25 2024-08-06 南京林业大学 Polydopamine-nanocellulose composite aerogel material, and preparation method and application thereof

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Application publication date: 20170915