CN106984282A - A kind of preparation method of the magnetic green substance adsorber of sulfydryl lignocellulosic montmorillonite Composite - Google Patents
A kind of preparation method of the magnetic green substance adsorber of sulfydryl lignocellulosic montmorillonite Composite Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of the magnetic green substance adsorber of sulfydryl lignocellulosic montmorillonite Composite, it is characterised in that with wheat stalk, ZnCl2, citric acid, N, N dimethylformamides, chitosan, epoxychloropropane, ethylenediamine, pyridine, triethylamine, sodium alginate, CaCl2、FeSO4、FeCl3, TGA, acetic anhydride, lignocellulosic, montmorillonite etc. be raw material.The present invention is modified in N, N dimethylformamides using citric acid, chitosan to biological particles;It is catalyzed with pyridine, cooperates with ethylenediamine cross-linking modified, prepare biomass adsorbent, with very high adsorption capacity;With FeSO4And FeCl3For raw material, the magnetic Fe of tool has been synthesized3O4, biological particles surface is carried on, and embedded using sodium alginate, prepare magnetic green substance adsorber;Obtain a kind of magnetic green substance adsorber of sulfydryl lignocellulosic montmorillonite Composite.
Description
Technical field
The present invention relates to a kind of preparation method of adsorbent, and in particular to a kind of sulfydryl lignocellulosic-montmorillonite Composite
Magnetic green substance adsorber preparation method.
Background technology
With the fast development of modern industry, the pollution of water resource is increasingly serious, wherein, most serious is heavy metal pollution
Problem.China possesses substantial amounts of biomass resource, wherein, agricultural wastes are a kind of renewable biomass resources, are prepared to
Various adsorbents, with the heavy metal ion pollutant in waste water of making a return journey, sewage.
Chen Yu is in its doctoral candidate's academic dissertation《The absorption research of biological material heavy metal pollutant copper》In, profit
It is raw material with rice straw, wheat straw, corn rice, four kinds of biomass of peanut shell, has been made up respectively of crushing, charing, modification primary
Material, carbon black materials and material modified three classes adsorbent, biomass raw material are after high temperature carbonization, from non-porous sorbing material
Become porous adsorbing material, them are have studied respectively to Cu2+Absorption.But it is not strong to there is adsorptivity, and adsorption range is too
Cross limitation.
Biomass material is passed through ZnCl by the present invention2Cooperate with microwave radiation modified so that fiber substance forms abundant
Hole, specific surface area greatly increases;In DMF, biological particles are entered using citric acid, chitosan
Row is modified, and citric acid can effectively improve the adsorption effect of adsorbent heavy metal ion, and chitosan heavy metal ion has
Certain capturing ability;Catalytic modification is carried out with pyridine, collaboration ethylenediamine is cross-linking modified, prepares biomass adsorbent, and it has
There is very high adsorption capacity;With FeSO4And FeCl3For raw material, the magnetic Fe of tool has been synthesized3O4, it is carried on biological particles table
Face, and embedded using sodium alginate, prepare magnetic green substance adsorber;Obtain a kind of sulfydryl lignocellulosic-Meng Tuo
The compound magnetic green substance adsorber of soil.
The content of the invention
The present invention solves the technical problem of provide a kind of magnetic bio of sulfydryl lignocellulosic-montmorillonite Composite
The preparation method of matter adsorbent, the adsorbent advantages of good adsorption effect prepared according to the technique, reproducibility are good.
The technical problems to be solved by the invention are realized using following technical scheme:
Wheat stalk 40-55, ZnCl2 2-5, citric acid 3-6, DMF 4-7, chitosan 2-4, epoxy chloropropionate
Alkane 2-5, ethylenediamine 3-5, pyridine 2-3, triethylamine 3-5, sodium alginate 3-5, CaCl2 2-4, FeSO4 4-5, FeCl3 3-4, mercapto
Guanidine-acetic acid 4-6, acetic anhydride 2-3, lignocellulosic 1-2, montmorillonite 3-5, acetic acid, dilute H2SO4, ammoniacal liquor, ethanol, distilled water, NaOH
The appropriate aqueous solution.
A kind of preparation method of the magnetic green substance adsorber of sulfydryl lignocellulosic-montmorillonite Composite, it is characterised in that
Carry out according to the following steps:
A. wheat stalk is rinsed well with water, in 100-110 DEG C of drying, crushes, sieves, collect diameter 0.1-0.5mm's
Biological particles;
B. by ZnCl2 1:2-4 is dissolved in water, resulting material in a is added thereto immersion 5-9h, then in 600-700W microwave
Lower activation 5-10min, adds acetic acid, dilute H2SO4, 100-110 DEG C is heated to reflux suction filtration after 2-3h, cooling, and alcohol washes, be washed to
Property, 55-110 DEG C of drying to constant weight;
C. citric acid is dissolved into DMF, with resulting material hybrid infusion 6-10h in b, is heated to 80-
120 DEG C of stirring 3-4h, suction filtration mixes filtrate with chitosan, and it is 8-10 to be heated to 50-80 DEG C of stirring 1-2h, tune pH, cool down,
Suction filtration, be washed to neutrality, by filter residue in 50-80 DEG C of drying, crush;
D. resulting material in c is mixed with epoxychloropropane, in after 90-110 DEG C of heating water bath stirring reaction 1-2h, adds second
Diamines, pyridine, triethylamine, constant temperature stirring reaction 2-3h adjust pH to neutrality, suction filtration, washing, alcohol are washed 3-5 times, in 50-60 DEG C of baking
Do to constant weight, obtain biomass adsorbent;
E. TGA, acetic anhydride, lignocellulosic are well mixed, 40-60 DEG C of water-bath 4-8h, 40-50 DEG C of drying,
1:25-35 is added in the NaOH aqueous solution, obtains A liquid;Into montmorillonite 1:30-40 adds water, is well mixed with A liquid, is heated to 60-
70 DEG C, stirring reaction 4-6h, product is washed to neutrality, 100-120 DEG C of dry 5-8h;
F. by FeSO4And FeCl3Add in distilled water, add resulting material, N in d, e2Stir, be slowly added dropwise under protection
Ammoniacal liquor, sodium alginate, CaCl2And distilled water, heating water bath is cooled to room temperature to 40-60 DEG C of reaction 2-3h, adjusts pH to neutrality,
Suction filtration, is washed 3-5 times, 60-80 DEG C of drying to constant weight obtains a kind of magnetic of sulfydryl lignocellulosic-montmorillonite Composite after grinding
Property biomass adsorbent.
The reaction mechanism of the present invention is as follows:
(1)Biomass material passes through ZnCl2Cooperate with microwave radiation modified so that fiber substance forms abundant hole, than
Surface area is greatly increased.
(2)It is citric acid good properties, cheap and easy to get, the adsorption effect of adsorbent heavy metal ion can be effectively improved,
In DMF, biological particles are modified using citric acid;Chitosan has good bio-compatible
Property, degradability, and rich in amino and hydroxyl, heavy metal ion has certain capturing ability.
(3)Catalytic modification is carried out with pyridine, collaboration ethylenediamine is cross-linking modified, prepares biomass adsorbent, and it has very
High adsorption capacity, ethylenediamine cross-linking method introduces more nitrogenous base functional groups, the surface of modified wheat stalk adsorbent
Introduce positively charged amine groups.
(4)Using TGA, acetic anhydride, lignocellulosic as raw material sulfydryl lignocellulosic has been made, by it in the present invention
Intercalation enters between the lamella of montmorillonite, improves adsorption effect of the adsorbent to heavy metal ions in wastewater, adsorption operations letter
Just, adsorbance is high.
(5)With FeSO4And FeCl3For raw material, the magnetic Fe of tool has been synthesized3O4, biological particles surface is carried on, and
Embedded using sodium alginate, prepare magnetic green substance adsorber, it has stronger magnetic, in the effect of externally-applied magnetic field
Under, separation of solid and liquid and recovery can be rapidly realized, heavy metal ion adsorbed subsequent treatment is simplified.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment
A kind of preparation method of the magnetic green substance adsorber of sulfydryl lignocellulosic-montmorillonite Composite, by following weight
The raw material of part (g) is made:
Wheat stalk 55, ZnCl2 5, citric acid 6, DMF 7, chitosan 4, epoxychloropropane 5, ethylenediamine 5,
Pyridine 3, triethylamine 5, sodium alginate 5, CaCl2 4, FeSO4 5, FeCl3 4, TGA 6, acetic anhydride 3, lignocellulosic 2,
Montmorillonite 5, acetic acid, dilute H2SO4, ammoniacal liquor, ethanol, distilled water, the NaOH aqueous solution it is appropriate.
A kind of preparation method of the magnetic green substance adsorber of sulfydryl lignocellulosic-montmorillonite Composite, it is characterised in that
Carry out according to the following steps:
A. wheat stalk is rinsed well with water, in 100-110 DEG C of drying, crushes, sieves, collect diameter 0.1-0.5mm's
Biological particles;
B. by ZnCl2 1:2 are dissolved in water, and resulting material in a is added thereto immersion 5h, then living under 600-700W microwave
Change 10min, add acetic acid, dilute H2SO4, 100-110 DEG C is heated to reflux suction filtration after 2h, cooling, and alcohol is washed, is washed to neutrality, 80-90
DEG C drying is to constant weight;
C. citric acid is dissolved into DMF, with resulting material hybrid infusion 8h in b, is heated to 90-110
DEG C stirring 3h, filtrate mix by suction filtration with chitosan, is heated to 70-80 DEG C and stirs 1h, tune pH is 8-9, cooling, suction filtration, washing
To neutral, by filter residue in 60-70 DEG C of drying, crushing;
D. resulting material in c is mixed with epoxychloropropane, in after 90-100 DEG C of heating water bath stirring reaction 1h, adds second two
Amine, pyridine, triethylamine, constant temperature stirring reaction 2h adjust pH to neutrality, suction filtration, washing, alcohol are washed 3 times, in 50-60 DEG C of drying to perseverance
Weight, obtains biomass adsorbent;
E. TGA, acetic anhydride, lignocellulosic are well mixed, 50-60 DEG C of water-bath 6h, 40-50 DEG C of drying, 1:
30 add in the NaOH aqueous solution, obtain A liquid;Into montmorillonite 1:35 add water, are well mixed with A liquid, are heated to 60-70 DEG C, stirred
Reaction 4h is mixed, product is washed to neutrality, 110-120 DEG C of dry 5h;
F. by FeSO4And FeCl3Add in distilled water, add resulting material, N in d, e2Stir, be slowly added dropwise under protection
Ammoniacal liquor, sodium alginate, CaCl2And distilled water, heating water bath is cooled to room temperature to 50-60 DEG C of reaction 2h, adjusts pH to neutrality, take out
Filter, is washed 3 times, 70-80 DEG C of drying to constant weight obtains a kind of magnetic green of sulfydryl lignocellulosic-montmorillonite Composite after grinding
Substance adsorber.
A kind of magnetic green material performance of the adsorbent inspection of sulfydryl lignocellulosic-montmorillonite Composite prepared by above-described embodiment
Survey result as follows:
The adsorbent is to Cr4+、Pb2+ 、Cu2+Maximal absorptive capacity respectively up to 251.3mg/g, 171.4mg/g, 56.1mg/g.
Claims (2)
1. a kind of preparation method of the magnetic green substance adsorber of sulfydryl lignocellulosic-montmorillonite Composite, it is characterised in that by
The raw material of following weight parts is made:
Wheat stalk 40-55, ZnCl2 2-5, citric acid 3-6, DMF 4-7, chitosan 2-4, epoxychloropropane
2-5, ethylenediamine 3-5, pyridine 2-3, triethylamine 3-5, sodium alginate 3-5, CaCl2 2-4, FeSO4 4-5, FeCl3 3-4, sulfydryl
Acetic acid 4-6, acetic anhydride 2-3, lignocellulosic 1-2, montmorillonite 3-5, acetic acid, dilute H2SO4, ammoniacal liquor, ethanol, distilled water, NaOH water
Appropriate solution.
2. a kind of system of the magnetic green substance adsorber of sulfydryl lignocellulosic-montmorillonite Composite according to claim 1
Preparation Method, it is characterised in that carry out according to the following steps:
A. wheat stalk is rinsed well with water, in 100-110 DEG C of drying, crushes, sieves, collect diameter 0.1-0.5mm's
Biological particles;
B. by ZnCl2 1:2-4 is dissolved in water, resulting material in a is added thereto immersion 5-9h, then in 600-700W microwave
Lower activation 5-10min, adds acetic acid, dilute H2SO4, 100-110 DEG C is heated to reflux suction filtration after 2-3h, cooling, and alcohol washes, be washed to
Property, 55-110 DEG C of drying to constant weight;
C. citric acid is dissolved into DMF, with resulting material hybrid infusion 6-10h in b, is heated to 80-
120 DEG C of stirring 3-4h, suction filtration mixes filtrate with chitosan, and it is 8-10 to be heated to 50-80 DEG C of stirring 1-2h, tune pH, cool down,
Suction filtration, be washed to neutrality, by filter residue in 50-80 DEG C of drying, crush;
D. resulting material in c is mixed with epoxychloropropane, in after 90-110 DEG C of heating water bath stirring reaction 1-2h, adds second
Diamines, pyridine, triethylamine, constant temperature stirring reaction 2-3h adjust pH to neutrality, suction filtration, washing, alcohol are washed 3-5 times, in 50-60 DEG C of baking
Do to constant weight, obtain biomass adsorbent;
E. TGA, acetic anhydride, lignocellulosic are well mixed, 40-60 DEG C of water-bath 4-8h, 40-50 DEG C of drying,
1:25-35 is added in the NaOH aqueous solution, obtains A liquid;Into montmorillonite 1:30-40 adds water, is well mixed with A liquid, is heated to 60-
70 DEG C, stirring reaction 4-6h, product is washed to neutrality, 100-120 DEG C of dry 5-8h;
F. by FeSO4And FeCl3Add in distilled water, add resulting material, N in d, e2Stir, be slowly added dropwise under protection
Ammoniacal liquor, sodium alginate, CaCl2And distilled water, heating water bath is cooled to room temperature to 40-60 DEG C of reaction 2-3h, adjusts pH to neutrality,
Suction filtration, is washed 3-5 times, 60-80 DEG C of drying to constant weight obtains a kind of magnetic of sulfydryl lignocellulosic-montmorillonite Composite after grinding
Property biomass adsorbent.
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CN107754773A (en) * | 2017-09-29 | 2018-03-06 | 周玲玲 | A kind of preparation method of epoxidation fiber manganese dioxide crossslinked sodium alginate microsphere adsorbing agent |
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CN114644782A (en) * | 2022-04-25 | 2022-06-21 | 黑龙江八一农垦大学 | Composite refined oil film based on corn straw nano-cellulose |
CN116809032A (en) * | 2023-07-03 | 2023-09-29 | 中国热带农业科学院南亚热带作物研究所 | Sulfhydryl modified chitosan porous microsphere and preparation method and application thereof |
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