CN104475044A - Method for preparing magnetic lignin adsorbent - Google Patents

Method for preparing magnetic lignin adsorbent Download PDF

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Publication number
CN104475044A
CN104475044A CN201410733512.9A CN201410733512A CN104475044A CN 104475044 A CN104475044 A CN 104475044A CN 201410733512 A CN201410733512 A CN 201410733512A CN 104475044 A CN104475044 A CN 104475044A
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China
Prior art keywords
lignin
magnetic
adsorbent
add
magnetic lignin
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Pending
Application number
CN201410733512.9A
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Chinese (zh)
Inventor
王海军
宋展欣
刘文涛
杨艳
王宁宁
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Jiangnan University
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Jiangnan University
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Priority to CN201410733512.9A priority Critical patent/CN104475044A/en
Publication of CN104475044A publication Critical patent/CN104475044A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid 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 physical properties
    • B01J20/28009—Magnetic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
    • C02F1/62—Heavy metal compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4837—Lignin

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention belongs to the technical field of water treatment, and particularly relates to an adsorbent for removing metal ions and a dye. The method is characterized in that lignin is adopted as a base body; epoxy chloropropane is adopted as a cross-linking agent; ferroferric oxide is adopted as a magnetic source; and diethylenetriamine, hexamethylenediamine, ethylenediamine and the like are adopted as aminating reagents. Compared with a traditional lignin adsorbent, the method has the characteristics that the adsorbent is easy to separate, can be repeatedly used, is beneficial to environmental protection and the like.

Description

A kind of method of magnetic lignin absorbent preparation
Technical field
The invention belongs to water-treatment technology field, be specifically related to a kind of adsorbent removing metal ion and dyestuff.
Background technology
The water resource of China is at space and skewness on the time; along with various production, the carrying out of life activity; water pollution exacerbates shortage of water resources; and industrial expansion adds the pressure of environmental protection in recent years; the multi industries with textile industry being wherein representative, with the color of dyestuff increase product, discharges one of very dark organic wastewater important sources becoming water environment pollution of color thus.In addition, the waste water containing heavy metal produced in the production process of the industry such as mine development, plating, chemical fertilizer, process hides, battery, papermaking, agricultural chemicals, if be discharged into directly or indirectly in environment, also can cause water pollutions in various degree.Therefore, the process of waste water is an important and large order.
Lignin is only second to cellulosic second largest natural polymer, and its basic structural unit is phenylpropyl alcohol alkyl.Because containing the various active groups such as phenolic hydroxyl group, alcoholic extract hydroxyl group, carbonyl, carboxyl, methoxyl group in its structure, have certain ion-exchange and absorption property, existing many researchers are to this has been research both at home and abroad, and achieve good effect.But Traditional Wood quality class adsorbent is unfavorable for recovery and reuse.
Summary of the invention
In order to solve lignin adsorbent recycling problem of the prior art, We conducted large quantifier elimination, found that and can adopt lignin composite magnetic, there is provided lignin adsorbent a magnetic response, make it be easy to be separated under magnetic fields, solve the problem of lignin adsorbent recycling.
Method provided by the invention is: (1) prepares magnetic lignin adsorbent matrix, preparation mass ratio is the lignin sodium hydroxide solution of 5 ~ 10%, add certain mass tri-iron tetroxide, ultrasonic 30min, add certain quantity of fluid paraffin after ultrasonic end, under stirring, add surfactant, add 1 ~ 5ml epoxychloropropane, react 2 ~ 5h at 50 ~ 90 DEG C, reaction terminates rear Magnetic Isolation vacuum drying.(2) magnetic lignin adsorbent based is modifies, and get previous step magnetic lignin adsorbent matrix 0.5g and add amination reagent, natrium carbonicum calcinatum, reaction 2 ~ 5h at 50 ~ 90 DEG C, Magnetic Isolation obtains product vacuum drying, is used for making adsorbent.
The present invention has the following advantages:
1. abundant raw material source, environmental protection;
2. the magnetic material lignin that prepared by the present invention effectively can remove the dyestuff in metal ion and waste water from dyestuff;
3. the magnetic material lignin that prepared by the present invention can be collected and be conducive to recycling under magnetic condition;
4. the magnetic material lignin that prepared by the present invention desorb can realize reusing of adsorbent in the basic conditions.
Magnetic lignin adsorbent dyestuff prepared by the present invention and the adsorption capacity of heavy metal ion and clearance, adopt static adsorptive method to detect, step is as follows:
Under room temperature, taking 20mg sample drops in 100ml conical flask, this conical flask adds metal ion solution under 25mL variable concentrations or dye solution more respectively, reconciling pH value is 2, at room temperature stirring and adsorbing 12h, Magnetic Isolation, atomic absorption spectrum or UV detector detect metal ion in solution or dye strength.According to formula (1) and (2) difference
Calculate adsorption capacity Q (mg/g) and the clearance q (%) of adsorbent:
Q＝(C o-C 1)V/m (1)，
q＝(C o-C 1)100％/C o(2)。
C o: initial concentration, mg/L C 1: absorption terminates concentration, mg/L V: liquor capacity, L m: add adsorbent mass, g.
Detailed description of the invention
The present invention's following examples illustrate, but the present invention is not limited to following embodiment, and under the prerequisite not departing from the described aim in front and back, change is included in technical scope of the present invention.
Embodiment 1
Implementation method is: 0.1g Fe 3o 4, add 5ml lignin NaOH solution (12wt%) ultrasonic 30min, add 20ml paraffin after ultrasonic end, 0.25g neopelex, add 2ml epoxychloropropane, react 3h at 60 DEG C, reaction terminates rear Magnetic Isolation vacuum drying.Get at previous step product adds 5ml diethylenetriamine, 12.5mg natrium carbonicum calcinatum 70 DEG C and react 3h, Magnetic Isolation obtains product vacuum drying, is used for making adsorbent.
Detect through static adsorptive method, this adsorbent 15mg is the azure dye absorption 12h of 300mg/L to 25mL initial concentration, and recording its remaining aniline blue concentration is 0.15mg/L, and its adsorption capacity is respectively 499.75mg/g, and clearance is 99.95%.
Detect through static adsorptive method, this adsorbent 35mg is the Cr of 100mg/L to 25mL initial concentration 6+solution absorption 12h, records its remaining Cr 6+ion concentration is 18.77mg/g, and its adsorption capacity is 58.01mg/g clearance is 81.21%.
Embodiment 2
Implementation method is: 0.1g Fe 3o 4, add 5ml lignin NaOH solution (12wt%) ultrasonic 30min, add 20ml paraffin after ultrasonic end, 0.25g neopelex, add 2ml epoxychloropropane, react 3h at 60 DEG C, reaction terminates rear Magnetic Isolation vacuum drying.Get at previous step product adds 4ml hexamethylene diamine, 12.5mg natrium carbonicum calcinatum 80 DEG C and react 3h, Magnetic Isolation obtains product vacuum drying, is used for making adsorbent.
Detect through static adsorptive method, this adsorbent 15mg is the azure dye absorption 12h of 300mg/L to 25mL initial concentration, and recording its remaining aniline blue concentration is 37.35mg/L, and its adsorption capacity is respectively 437.75mg/g, and clearance is 87.55%.
Detect through static adsorptive method, this adsorbent 35mg is the Cr of 100mg/L to 25mL initial concentration 6+solution absorption 12h, records its remaining Cr 6+ion concentration is 27.51mg/g, and its adsorption capacity is 51.78mg/g clearance is 72.49%.

Claims (5)

1. a method for magnetic lignin absorbent preparation, has following method to prepare:
(1) magnetic lignin adsorbent matrix is prepared, preparation mass ratio is the lignin sodium hydroxide solution of 5 ~ 10%, add certain mass tri-iron tetroxide, ultrasonic 30min, add certain quantity of fluid paraffin after ultrasonic end, under stirring, add surfactant, add 1 ~ 5ml epoxychloropropane, react 2 ~ 5h at 50 ~ 90 DEG C, reaction terminates rear Magnetic Isolation vacuum drying.
(2) magnetic lignin adsorbent based is modifies, gets that previous step magnetic lignin adsorbent matrix 0.5g adds aminating agent, reaction 2 ~ 5h at 50 ~ 90 DEG C, and Magnetic Isolation obtains product vacuum drying, is used for making adsorbent.
2. the method for a kind of magnetic lignin absorbent preparation according to claim 1, is characterized in that the surfactant described is the surfactants such as neopelex, Tween 80, polysorbate60, class of department 60.
3. the method for a kind of magnetic lignin absorbent preparation according to claim 1, is characterized in that the addition of described surfactant is 1 ~ 10% of mixed solution quality.
4. the method for a kind of magnetic lignin absorbent preparation according to claim 1, is characterized in that the concentration of NaOH is 5 ~ 20% (wt%).
5. the method for a kind of magnetic lignin absorbent preparation according to claim 1, is characterized in that amination reagent is the aminated compounds such as diethylenetriamine, ethylenediamine, hexamethylene diamine.
CN201410733512.9A 2014-12-04 2014-12-04 Method for preparing magnetic lignin adsorbent Pending CN104475044A (en)

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105854822A (en) * 2016-04-21 2016-08-17 华南理工大学 Method for preparing Cu<2+> adsorbent from corn stalk enzymolysis residue and application of Cu<2+> adsorbent
CN106698581A (en) * 2017-01-17 2017-05-24 河北工业大学 Adsorption treatment method for cationic dye
CN107262054A (en) * 2017-07-28 2017-10-20 江苏大学 A kind of preparation method and applications of magnetic lignin base adsorbent
CN108057427A (en) * 2017-12-14 2018-05-22 湖南科技大学 A kind of solid magnetic separation of heavy metal ions material and preparation method thereof
CN108339523A (en) * 2018-01-23 2018-07-31 天津大学 The preparation and application of lignin or the lignin-modified magnetic nanometer adsorbent of amido
CN108636357A (en) * 2018-06-07 2018-10-12 石梦成 A kind of use in waste water treatment cross-linking type graphite oxide aerogel and preparation method thereof
CN108686628A (en) * 2018-05-28 2018-10-23 中国林业科学研究院林产化学工业研究所 A kind of preparation method of the water-oil separating recyclable aeroge of waste paper base
CN109126746A (en) * 2018-10-17 2019-01-04 北京林业大学 A kind of preparation method of magnetism lignosulfonates adsorbent material
CN110115983A (en) * 2019-05-20 2019-08-13 湖南科技大学 A kind of Beta-cyclodextrin-based chelating decolorizing and absorbing material of solid and preparation method thereof
CN110115984A (en) * 2019-05-20 2019-08-13 湖南科技大学 A kind of Beta-cyclodextrin-based cross-linked polymer adsorbent material of magnetism and preparation method thereof
CN110115985A (en) * 2019-05-20 2019-08-13 湖南科技大学 A kind of Beta-cyclodextrin-based cross-linked polymer adsorbent material and preparation method thereof
CN110115982A (en) * 2019-05-20 2019-08-13 湖南科技大学 A kind of Beta-cyclodextrin-based chelating decolorizing and absorbing material of magnetism and preparation method thereof
CN111744460A (en) * 2020-07-16 2020-10-09 中国林业科学研究院林产化学工业研究所 Triazine type lignin-based magnetic adsorption material and preparation method thereof

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CN103585956A (en) * 2013-11-25 2014-02-19 西南交通大学 Preparation method for magnetic lignin-based activated carbon

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CN103585956A (en) * 2013-11-25 2014-02-19 西南交通大学 Preparation method for magnetic lignin-based activated carbon

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Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105854822A (en) * 2016-04-21 2016-08-17 华南理工大学 Method for preparing Cu<2+> adsorbent from corn stalk enzymolysis residue and application of Cu<2+> adsorbent
CN106698581B (en) * 2017-01-17 2020-05-05 河北工业大学 Adsorption treatment method of cationic dye
CN106698581A (en) * 2017-01-17 2017-05-24 河北工业大学 Adsorption treatment method for cationic dye
CN107262054A (en) * 2017-07-28 2017-10-20 江苏大学 A kind of preparation method and applications of magnetic lignin base adsorbent
CN108057427A (en) * 2017-12-14 2018-05-22 湖南科技大学 A kind of solid magnetic separation of heavy metal ions material and preparation method thereof
CN108057427B (en) * 2017-12-14 2020-05-26 湖南科技大学 Solid magnetic heavy metal ion separation material and preparation method thereof
CN108339523A (en) * 2018-01-23 2018-07-31 天津大学 The preparation and application of lignin or the lignin-modified magnetic nanometer adsorbent of amido
CN108686628A (en) * 2018-05-28 2018-10-23 中国林业科学研究院林产化学工业研究所 A kind of preparation method of the water-oil separating recyclable aeroge of waste paper base
CN108636357A (en) * 2018-06-07 2018-10-12 石梦成 A kind of use in waste water treatment cross-linking type graphite oxide aerogel and preparation method thereof
CN109126746A (en) * 2018-10-17 2019-01-04 北京林业大学 A kind of preparation method of magnetism lignosulfonates adsorbent material
CN110115983A (en) * 2019-05-20 2019-08-13 湖南科技大学 A kind of Beta-cyclodextrin-based chelating decolorizing and absorbing material of solid and preparation method thereof
CN110115984A (en) * 2019-05-20 2019-08-13 湖南科技大学 A kind of Beta-cyclodextrin-based cross-linked polymer adsorbent material of magnetism and preparation method thereof
CN110115985A (en) * 2019-05-20 2019-08-13 湖南科技大学 A kind of Beta-cyclodextrin-based cross-linked polymer adsorbent material and preparation method thereof
CN110115982A (en) * 2019-05-20 2019-08-13 湖南科技大学 A kind of Beta-cyclodextrin-based chelating decolorizing and absorbing material of magnetism and preparation method thereof
CN110115984B (en) * 2019-05-20 2022-03-22 湖南科技大学 Magnetic cyclodextrin-based cross-linked polymer adsorption material and preparation method thereof
CN110115983B (en) * 2019-05-20 2022-03-22 湖南科技大学 Solid cyclodextrin-based chelating and decolorizing adsorption material and preparation method thereof
CN110115985B (en) * 2019-05-20 2022-03-22 湖南科技大学 Cyclodextrin-based cross-linked polymer adsorption material and preparation method thereof
CN110115982B (en) * 2019-05-20 2022-03-25 湖南科技大学 Magnetic cyclodextrin-based chelating and decolorizing adsorption material and preparation method thereof
CN111744460A (en) * 2020-07-16 2020-10-09 中国林业科学研究院林产化学工业研究所 Triazine type lignin-based magnetic adsorption material and preparation method thereof

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Application publication date: 20150401