CN109675529A - Modified jute adsorbent of a kind of magnetic and preparation method thereof - Google Patents

Modified jute adsorbent of a kind of magnetic and preparation method thereof Download PDF

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Publication number
CN109675529A
CN109675529A CN201910035472.3A CN201910035472A CN109675529A CN 109675529 A CN109675529 A CN 109675529A CN 201910035472 A CN201910035472 A CN 201910035472A CN 109675529 A CN109675529 A CN 109675529A
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China
Prior art keywords
jute
adsorbent
preparation
magnetic
modified
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CN201910035472.3A
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Chinese (zh)
Inventor
邓灿辉
粟建光
陈基权
杨泽茂
戴志刚
唐蜻
许英
程超华
刘禅
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Institute of Bast Fiber Crops of CAAS
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Institute of Bast Fiber Crops of CAAS
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Priority to CN201910035472.3A priority Critical patent/CN109675529A/en
Publication of CN109675529A publication Critical patent/CN109675529A/en
Pending legal-status Critical Current

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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
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0225Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • B01J20/0229Compounds of Fe
    • 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
    • B01J20/28002Solid 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
    • B01J20/28009Magnetic properties
    • 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
    • C02F1/286Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • C02F2101/22Chromium or chromium compounds, e.g. chromates

Abstract

The present invention relates to industrial waste water treatment, in particular to a kind of modified jute adsorbent of magnetic and preparation method thereof.The jute sorbent preparation method includes: to be passed through N2Under the conditions of, jute powder is dispersed in containing Fe2+And Fe3+Aqueous solution in, adjust pH to 8~10,2~6h reacted at 70~90 DEG C, collecting reaction product is washed with water to neutrality, and freeze-drying obtains jute adsorbent.Experiment shows that the modified jute adsorbent of magnetic prepared by the present invention can effectively remove the heavy metal chromium in waste water, and the adsorption capacity to chromium is 2.7 times or more of unmodified jute adsorbent.In addition, preparing adsorbent by raw material of jute, abundance is low in cost, and preparation method is simple, can effectively realize mass production, can be used for extensive heavy metal in water pollution of chromium purification.

Description

Modified jute adsorbent of a kind of magnetic and preparation method thereof
Technical field
The present invention relates to industrial waste water treatment more particularly to a kind of modified jute adsorbent of magnetic and its preparation sides Method.
Background technique
Heavy metal pollution caused by industrial production and mineral mining has become most one of difficult problem in wastewater treatment.? In each heavy metal species, chromium becomes one of most intractable heavy metal pollution due to having high toxicity, carcinogenicity and teratogenesis.Cr (III) and the most common two kinds of chemical valences of Cr (VI) all chromiums, wherein Cr (VI) has more solubility, mobility, mutagenicities And toxicity, and toxicity is 100 times of Cr (III).For Cr (VI) once entering human body, will cause to human organ, DNA etc. can not The damage retrieved.Therefore, pollution of chromium improvement in Cr (VI) pollution control be we work in the most important thing.According to statistics, China is over the years by the largely not up to electroplating wastewater direct emissions of discharge standards, and the chromium that air storage is not disposed largely Slag.These chromium slags pass through the leaching and percolation of rainwater, and heavy metal chromium enters soil, penetrates into underground water or shallow water storage Layer, causes the economic loss for being difficult to estimate.Therefore, the method for taking economical and efficient administers pollution of chromium, becomes our environmental improvements In important process.
Absorption method receives significant attention due to being a kind of more efficient, economy process for treating heavy-metal waste water.Work at present It is active carbon that most adsorbents is applied in industry, but it is expensive, regeneration rate is low.Jute is Tiliaceae (Tiliaceae) yellow Fiber crops belong to (Corchorus) annual herb plant, are a kind of abundance, cheap natural reproducible resource.In recent years The study found that each position of jute, including tossa, jute stalk core and roundpod jute leaf are because containing fiber-like and stickiness polysaccharide object Matter has certain absorption property to heavy metal chromium, cadmium, copper, lead etc..Therefore the huge sum of money accessory in jute removal waste water is utilized There is cheap, efficient and environmental-friendly practical significance.
But has the effective component of chelation limited in heavy metal in jute, also have to the adsorption capacity of heavy metal ion Limit, and the good dispersion of jute powder in aqueous solution are difficult to separate from aqueous solution after so that it is adsorbed heavy metal.
Summary of the invention
In view of this, the purpose of the present invention is to provide modified jute adsorbent of a kind of magnetic and preparation method thereof, this method The modified jute adsorbent of the magnetic of preparation has good adsorption effect to heavy metal ion, and is easy to separate from water body, no It will cause secondary pollution.
In order to achieve the object of the present invention, the present invention adopts the following technical scheme:
The present invention provides a kind of preparation method of modified jute adsorbent of magnetic, comprising:
It is being passed through N2Under the conditions of, jute powder is dispersed in containing Fe3+And Fe2+Aqueous solution in, obtain mixed liquor;
Mixed liquor pH value to 2~6h of reaction, collecting reaction product at 8~10,70~90 DEG C is adjusted to wash with water into Property, freeze-drying obtains the modified jute adsorbent of magnetic.
In some embodiments, the partial size of jute powder is 100~500 μm.
In some embodiments, it after the jute powder is by fresh jute natural drying, is washed with deionized water, in 50 ~100 DEG C of drying, grinding obtain.
In certain embodiments, when preparing jute powder, after natural drying by fresh jute, first it is truncated into 2~3cm Then segment is washed with deionized water again.
In some embodiments, the jute is tossa, jute stalk core or roundpod jute leaf.
In some embodiments, Fe in the mixed liquor2+With Fe3+Molar ratio be 1:1.5~2.In some specific realities It applies in example, Fe2+With Fe3+Molar ratio be 1:1.5,1:1.6 or 1:2.
In some embodiments, the jute powder and Fe3+Mass ratio be 1:1~5.
In some embodiments, the jute powder and Fe3+Mass ratio be 1:1.26~4.48.
In certain embodiments, jute powder and Fe3+Mass ratio are as follows: 1:1.26,1:1.68,1:2.52 or 1: 4.48。
In some embodiments, the regulator that the adjusting pH is used is 25% ammonium hydroxide.
The present invention also provides the modified jute adsorbents of the magnetic being prepared by preparation method of the present invention.
The present invention also provides the modified jute adsorbents of the magnetic in the application for adsorbing heavy metal ions in wastewater.Some In embodiment, the heavy metal ion is hexavalent chromium.
The preparation method of jute adsorbent provided by the invention includes: to be passed through N2Under the conditions of, jute powder is uniformly divided It is dispersed in containing Fe3+And Fe2+Aqueous solution in, obtain mixed liquor;Mixed liquor pH value is adjusted to reacting 2~6h at 8~10,70~90 DEG C, Collecting reaction product is washed with water to neutrality, freeze-drying, obtains the modified jute adsorbent of magnetic.Experiments have shown that prepared by the present invention The modified jute adsorbent of magnetic can effectively remove the heavy metal chromium in waste water, the adsorption capacity to chromium is unmodified jute absorption 2.7 times or more of agent.In addition, preparing adsorbent by raw material of jute, abundance is low in cost, and preparation method is simple, It can effectively realize mass production, and adsorbent is easy to separate from water body not will cause secondary pollution, can be used for extensive water The purification of body heavy metal chromium pollution.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technical description to be briefly described.
Fig. 1 is result figure of the modified jute adsorbent of magnetic to the absorption of Cr (VI) solution, separation of the embodiment of the present invention 1~4;
Fig. 2 is that the magnetic of the embodiment of the present invention 1~4 is modified the jute stalk core powder of jute adsorbent and control group 1 to a huge sum of money Belong to the histogram of ion Cr (VI) adsorption effect.
Specific embodiment
The invention discloses modified jute adsorbents of a kind of magnetic and preparation method thereof, and those skilled in the art can use for reference this Literary content, is suitably modified realization of process parameters.In particular, it should be pointed out that all similar substitutions and modifications are to art technology It is it will be apparent that they are considered as being included in the present invention for personnel.Method and application of the invention has passed through preferably Embodiment is described, related personnel obviously can not depart from the content of present invention, in spirit and scope to side as described herein Method and application are modified or appropriate changes and combinations, carry out implementation and application the technology of the present invention.
To the explanation of the disclosed embodiments, enable those skilled in the art to implement or use the present invention.To this A variety of modifications of a little embodiments will be readily apparent to those skilled in the art, as defined herein general Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, the present invention will not It can be intended to be limited to the embodiments shown herein, and be to fit to consistent with the principles and novel features disclosed in this article Widest scope.
The test material that the present invention uses is all common commercially available product, can all be bought in market.
Below with reference to embodiment, the present invention is further explained:
Embodiment 1
(1) by after the jute stalk core natural drying of fresh harvest, it is truncated into 2~3cm, is washed with deionized water, 80 DEG C of bakings It is dry, required jute stalk core powder is obtained after smashing it through 60 meshes;
(2) it is being passed through N2Under the conditions of, 1g jute stalk core powder is dispersed in 150mL containing Fe3+And Fe2+Aqueous solution in (its In use FeCl3·6H2O prepares to obtain Fe3+Concentration in aqueous solution is 0.15mol/L, uses FeSO4·7H2O prepares to obtain Fe2+ Concentration in aqueous solution is 0.1mol/L, and jute powder and Fe3+Mass ratio be 1:1.26), 70 DEG C are mixed evenly Afterwards, after the ammonium hydroxide of 4mL25% is added, the reaction was continued at 70 DEG C 3h separates and collects product with magnet, and cleaned with deionized water To neutrality, freeze-drying is for 24 hours to get the modified jute adsorbent of magnetic.
Embodiment 2
(1) by after the jute stalk core natural drying of fresh harvest, it is truncated into 2~3cm, is washed with deionized water, 80 DEG C of bakings It is dry, required jute stalk core powder is obtained after smashing it through 60 meshes;
(2) it is being passed through N2Under the conditions of, 2g jute stalk core powder is dispersed in 150mL containing Fe3+And Fe2+Aqueous solution in (its In use FeCl3·6H2O prepares to obtain Fe3+Concentration in aqueous solution is 0.4mol/L, uses FeSO4·7H2O prepares to obtain Fe2+ Concentration in aqueous solution is 0.25mol/L, and jute powder and Fe3+Mass ratio be 1:1.68), 70 DEG C are mixed evenly Afterwards, after the ammonium hydroxide of 12mL25% is added, the reaction was continued at 70 DEG C 3h separates and collects product with magnet, and clear with deionized water It is washed till neutrality, freeze-drying is for 24 hours to get the modified jute adsorbent of magnetic.
Embodiment 3
(1) by after the jute stalk core natural drying of fresh harvest, it is truncated into 2~3cm, is washed with deionized water, 80 DEG C of bakings It is dry, required jute stalk core powder is obtained after smashing it through 60 meshes;
(2) it is being passed through N2Under the conditions of, 1.2g jute stalk core powder is dispersed in 150mL containing Fe3+And Fe2+Aqueous solution in (wherein use FeCl3·6H2O prepares to obtain Fe3+Concentration in aqueous solution is 0.3mol/L, uses FeSO4·7H2O prepares to obtain Fe2+Concentration in aqueous solution is 0.15mol/L, and jute powder and Fe3+Mass ratio be 1:2.52), 70 DEG C mixing After uniformly, after the ammonium hydroxide of 10mL25% is added, the reaction was continued at 70 DEG C 3h separates and collects product with magnet, and use deionization Water is cleaned to neutrality, and freeze-drying is for 24 hours to get the modified jute adsorbent of magnetic.
Embodiment 4
(1) by after the jute stalk core natural drying of fresh harvest, it is truncated into 2~3cm, is washed with deionized water, 80 DEG C of bakings It is dry, required jute stalk core powder is obtained after smashing it through 60 meshes;
(2) it is being passed through N2Under the conditions of, 1.5g jute stalk core powder is dispersed in 150mL containing Fe3+And Fe2+Aqueous solution in (wherein use FeCl3·6H2O prepares to obtain, Fe3+Concentration in aqueous solution is 0.8mol/L, uses FeSO4·7H2O prepares to obtain Fe2+Concentration in aqueous solution is 0.5mol/L, and jute powder and Fe3+Mass ratio be 1:4.48), 70 DEG C mixing After uniformly, after the ammonium hydroxide of 25mL25% is added, the reaction was continued at 70 DEG C 3h separates and collects product with magnet, and use deionization Water is cleaned to neutrality, and freeze-drying is for 24 hours to get the modified jute adsorbent of magnetic.
Embodiment 5
The preparation of 1 sample of control group: after the jute stalk core natural drying of fresh harvest, being truncated into 2~3cm, spend from Sub- water is cleaned, 80 DEG C of drying, smash it through after 60 meshes needed for jute stalk core powder, as a control group 1.
The modified jute of magnetic prepared by 1 sample of control group, embodiment 1, embodiment 2, embodiment 3 and embodiment 4 is as suction Attached dose, Staticadsorption experiment is carried out to Cr (VI).
The potassium bichromate solution 100mL that the mass concentration of Cr (VI) is 100mg/L is taken, with the HNO of 0.5M3With 0.5M's It is 6.0 that NaOH, which adjusts Cr (VI) pH value of solution,;It is separately added into 1 sample of 0.1g control group thereto, embodiment 1, embodiment 2, implements The modified jute adsorbent of magnetic prepared by example 3 and embodiment 4, is placed on shaking table and is shaken under the conditions of 25 DEG C with the revolving speed of 150rpm/min Swing reaction for 24 hours;After respectively adsorbent and Cr (VI) solution being separated with magnet separation method with centrifugation, take out 0.5mL supernatant, With deionized water constant volume to 50mL, and Cr in filtrate is measured under 540nm wavelength with two hydrazine spectrophotometry of diphenyl phosphinylidyne (VI) concentration, and jute stalk core and the modified jute of magnetic are calculated to the adsorption capacity of Cr (VI), sample absorption, separating resulting are shown in figure 1, adsorption capacity calculated result is shown in Fig. 2.Wherein, the left side Fig. 1 is that the modified jute adsorbent of magnetic of the embodiment of the present invention 1~2 is dispersed in State diagram in Cr (VI) solution, the right side Fig. 1 are to be divided the modified jute adsorbent of magnetic and Cr (VI) solution with magnet after reacting From result figure.
As shown in Figure 1, the modified jute adsorbent of magnetic provided by the invention has certain magnetic saturation intensity, just using magnet It can be separated from water body, not will cause secondary pollution.
As shown in Figure 2, when reaching adsorption equilibrium, the modified Huang of magnetic of control group 1, embodiment 2, embodiment 3 and embodiment 4 Fiber crops are respectively 7.45,26.54,30.58,28.78 and 20.26mg/g to the adsorption capacity of heavy metal Cr (VI).The present invention 1~4 Magnetic modified adsorbent 1 be significantly increased compared to the control group to the adsorption capacity of heavy metal Cr (VI), wherein embodiment 2 prepare The modified jute of magnetic in jute powder and Fe3+Adsorption capacity highest under optimal proportion, adsorption effect are best.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (10)

1. a kind of preparation method of the modified jute adsorbent of magnetic characterized by comprising
It is being passed through N2Under the conditions of, jute powder is dispersed in containing Fe3+And Fe2+Aqueous solution in, obtain mixed liquor;
Mixed liquor pH value is adjusted to 2~6h of reaction at 8~10,70~90 DEG C, collecting reaction product is washed with water to neutrality, cold Dry, the modified jute adsorbent of acquisition magnetic is lyophilized.
2. preparation method according to claim 1, which is characterized in that the partial size of the jute powder is 100~500 μm.
3. preparation method according to claim 1, which is characterized in that the jute powder is by fresh jute natural drying Afterwards, it is washed with deionized water, is obtained in 50~100 DEG C of drying, grinding.
4. preparation method according to claim 3, which is characterized in that the jute is tossa, jute stalk core or Huang Sesame slices.
5. preparation method according to claim 1, which is characterized in that Fe in the mixed liquor2+With Fe3+Molar ratio be 1: 1.5~2.
6. preparation method according to claim 1, which is characterized in that the jute powder and Fe3+Mass ratio be 1:1~ 5。
7. preparation method according to claim 1, which is characterized in that it is described adjust the regulator that uses of mixed liquor pH value for 25% ammonium hydroxide.
8. the modified jute adsorbent of the magnetic that preparation method described in claim 1~7 is prepared.
9. the modified jute adsorbent of magnetic according to any one of claims 8 is in the application of absorption heavy metal ions in wastewater.
10. application according to claim 9, which is characterized in that the heavy metal ion is hexavalent chromium.
CN201910035472.3A 2019-01-15 2019-01-15 Modified jute adsorbent of a kind of magnetic and preparation method thereof Pending CN109675529A (en)

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Cited By (1)

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Application publication date: 20190426