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 PDF

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CN106984282A
CN106984282A CN201710307471.0A CN201710307471A CN106984282A CN 106984282 A CN106984282 A CN 106984282A CN 201710307471 A CN201710307471 A CN 201710307471A CN 106984282 A CN106984282 A CN 106984282A
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lignocellulosic
sulfydryl
water
montmorillonite
drying
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葛文双
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Fengtai Shuangli Biological Technology Co Ltd
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    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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    • 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
    • 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
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • 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
    • C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • 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
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/46—Materials comprising a mixture of inorganic and organic materials
    • 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
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    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F2101/22—Chromium or chromium compounds, e.g. chromates

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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

A kind of system of the magnetic green substance adsorber of sulfydryl lignocellulosic-montmorillonite Composite Preparation Method
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.
CN201710307471.0A 2017-05-04 2017-05-04 A kind of preparation method of the magnetic green substance adsorber of sulfydryl lignocellulosic montmorillonite Composite Pending CN106984282A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107555521A (en) * 2017-10-27 2018-01-09 卢伟 A kind of heavy metal-polluted water process multiporous biological matter microballoon and preparation method thereof
CN107722991A (en) * 2017-10-31 2018-02-23 中国环境科学研究院 A kind of heavy metal-polluted soil pollution of chromium repair materials and preparation method and application
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
CN107935064A (en) * 2017-10-30 2018-04-20 安徽铭能保温科技有限公司 A kind of brewery's residual water removes turbid inorganic agent and preparation method thereof
CN109647353A (en) * 2019-01-30 2019-04-19 刘华 A kind of heavy metal containing sewage composite treating agent and its preparation method and application
CN110624510A (en) * 2019-09-11 2019-12-31 合肥学院 Composite adsorbent and method for treating chrome black-containing T printing and dyeing wastewater by using same
CN111018016A (en) * 2019-12-12 2020-04-17 清华大学 Heavy metal sewage treatment agent
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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JPH0780294A (en) * 1993-09-09 1995-03-28 Mitsubishi Chem Corp Composite 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
CN107555521B (en) * 2017-10-27 2018-07-03 南京苏环环境互联科技有限公司 A kind of heavy metal-polluted water process multiporous biological matter microballoon and preparation method thereof
CN107555521A (en) * 2017-10-27 2018-01-09 卢伟 A kind of heavy metal-polluted water process multiporous biological matter microballoon and preparation method thereof
CN107935064A (en) * 2017-10-30 2018-04-20 安徽铭能保温科技有限公司 A kind of brewery's residual water removes turbid inorganic agent and preparation method thereof
CN107722991A (en) * 2017-10-31 2018-02-23 中国环境科学研究院 A kind of heavy metal-polluted soil pollution of chromium repair materials and preparation method and application
CN109647353B (en) * 2019-01-30 2022-01-04 常州市新未来化工有限公司 Heavy metal sewage composite treating agent and preparation method and application thereof
CN109647353A (en) * 2019-01-30 2019-04-19 刘华 A kind of heavy metal containing sewage composite treating agent and its preparation method and application
CN110624510A (en) * 2019-09-11 2019-12-31 合肥学院 Composite adsorbent and method for treating chrome black-containing T printing and dyeing wastewater by using same
CN110624510B (en) * 2019-09-11 2021-10-29 合肥学院 Composite adsorbent and method for treating chrome black-containing T printing and dyeing wastewater by using same
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CN116809032B (en) * 2023-07-03 2024-06-04 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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Application publication date: 20170728