CN105536752A - Preparation method of magnetic montmorillonite composite granular adsorbent - Google Patents
Preparation method of magnetic montmorillonite composite granular adsorbent Download PDFInfo
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- CN105536752A CN105536752A CN201510919609.3A CN201510919609A CN105536752A CN 105536752 A CN105536752 A CN 105536752A CN 201510919609 A CN201510919609 A CN 201510919609A CN 105536752 A CN105536752 A CN 105536752A
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
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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
- B01J20/28—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
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- 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
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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
- 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
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The invention relates to a preparation method of a magnetic montmorillonite composite granular adsorbent, and belongs to the field of adsorption material preparation. Aiming at the problems that montmorillonite is taken as an adsorbent, has relatively poor adsorption capacity and needs to be compounded and modified at present, an iron ion mixed solution is prepared from ferric chloride and ferrous chloride, then the iron ion mixed solution is oxidized under the protection of nitrogen to prepare a ferroferric oxide magnetic fluid mixed solution, and the magnetic montmorillonite composite granular adsorbent is prepared by compounding montmorillonite with the ferroferric oxide magnetic fluid mixed solution. Montmorillonite is screened and modified to prepare the granular adsorbent, and the adsorption effect of the granular adsorbent on heavy metal ions reaches more than or equal to 90%; and moreover, with montmorillonite for preparing the adsorbent, the cost is reduced, and the method has the advantages of green environmental protection and no pollution.
Description
Technical field
The present invention relates to a kind of preparation method of magnetic montmorillonite Composite granule adsorbent, belong to sorbing material preparation field.
Background technology
Along with increasingly sharpening of heavy metal wastewater thereby environmental pollution, the heavy metal ion removed in water becomes the problem needing solution badly.Absorption method is the effective ways of process heavy metal wastewater thereby, and in recent years, clay mineral and trade waste are used for sewage purification as new adsorbent becomes study hotspot.Wherein, montmorillonite because of wide material sources, cheap and absorption property is good and be considered to extremely potential.
The absorption of imvite has lot of advantages, therefore, in recent years, resource scarcity is by being used widely imvite in environmental improvement heavy metal process row, and the regenerative agent of preparation magnetic montmorillonite Composite granule adsorbent and high reproducibility becomes current particularly important research point.
Summary of the invention
Technical problem to be solved by this invention: for adopting imvite as adsorbent at present; adsorption capacity is poor and need to the problem of its compound and modification; provide one and prepare iron ion mixed liquor by iron chloride and frerrous chloride; subsequently it is carried out under nitrogen protection oxidation and be prepared into oxidation three body magnetic fluid mixed liquor; by it, compound is carried out to imvite and prepare a kind of magnetic montmorillonite Composite granule adsorbent, can effectively adsorb heavy metal in waste water particle and process.
For solving the problems of the technologies described above, the present invention adopts technical scheme as described below to be:
(1) 1:1 by volume, the ferric chloride solution of 0.45mol/L and the solution of ferrous chloride of 0.25mol/L are added in the there-necked flask of 150mL, subsequently under 500 ~ 600r/min rotating speed, to its overtime work mixing 10 ~ 15min, be prepared into iron ion mixed liquor;
(2) after mixing to be mixed completes, 3:1 in mass ratio, the ammonia spirit of 1.25mol/L is added in iron ion mixed liquor, after solution blackening, to its logical nitrogen protection and to its continuation stirring 25 ~ 30min, subsequently to its standing separation 2 ~ 3min, there-necked flask is moved near magnetic field and carry out Magneto separate process 15 ~ 20min;
(3) treat that solution is clarified completely, it is filtered and collects filter residue, and after spending deionized water 3 ~ 5 times, by solid-to-liquid ratio 1:10, be dispersed in deionized water, the 25 ~ 30min of ultrasonic wave added vibration subsequently, be prepared into four oxidation three body magnetic fluid mixed liquors, for subsequent use;
(4) imvite of drying is placed in high pressure milling device, to its 10 ~ 15min sieving of milling, be prepared into 60 ~ 80 object montmorillonite particles, regrading subsequently, rinse by deionized water while screening, to be rinsed complete after, to be placed in 60 ~ 80 DEG C of baking ovens dry 6 ~ 8h, to collect to obtain 150 ~ 160 object montmorillonite particles;
(5) count by weight, choose four oxidation three body magnetic fluid mixed liquors prepared by the montmorillonite particle of the above-mentioned preparation of 45 ~ 65 parts, the epoxy resin of 10 ~ 15 parts and 25 ~ 40 parts of steps (3), 10 ~ 15min is uniformly mixed under being placed on 600 ~ 800r/min, still aging 20 ~ 24h subsequently, it is filtered and collects filter residue, dry 6 ~ 8h in 60 ~ 80 DEG C of baking ovens, natural wind dry doubling calcination activation 2 ~ 3h at 300 ~ 400 DEG C subsequently, naturally cool to room temperature, a kind of magnetic montmorillonite Composite granule adsorbent can be prepared into.
Application process of the present invention is: getting magnetic montmorillonite Composite granule adsorbent that 20 ~ 40g obtains, to be carried on aperture be on the screen cloth of 20 μm, being holded up by screen cloth is placed in wastewater disposal basin, one is laid every 50 ~ 60cm, pass into the cadmium wastewater that mass concentration is 20 ~ 200mg/L, stop 6 ~ 8h, recording cadmium ion ionic adsorption capacity is 18 ~ 190mg/g, and adsorption rate reaches more than 90%.
The present invention is compared with additive method, and Advantageous Effects is:
(1) the present invention prepares granule adsorbent by imvite screening modification, and heavy metal ionic adsorption effect reaches more than 90%;
(2) prepare adsorbent by imvite, reduce costs, environmental protection is pollution-free.
Detailed description of the invention
First 1:1 by volume, is added in the there-necked flask of 150mL by the ferric chloride solution of 0.45mol/L and the solution of ferrous chloride of 0.25mol/L, subsequently under 500 ~ 600r/min rotating speed, to its overtime work mixing 10 ~ 15min, is prepared into iron ion mixed liquor; After mixing to be mixed completes, 3:1 in mass ratio, the ammonia spirit of 1.25mol/L is added in iron ion mixed liquor, after solution blackening, to its logical nitrogen protection and to its continuation stirring 25 ~ 30min, subsequently to its standing separation 2 ~ 3min, there-necked flask is moved near magnetic field and carry out Magneto separate process 15 ~ 20min; Treat that solution is clarified completely, filter and collect filter residue to it, and after spending deionized water 3 ~ 5 times, by solid-to-liquid ratio 1:10, be dispersed in deionized water, the 25 ~ 30min of ultrasonic wave added vibration subsequently, is prepared into four oxidation three body magnetic fluid mixed liquors, for subsequent use; The imvite of drying is placed in high pressure milling device, to its 10 ~ 15min sieving of milling, be prepared into 60 ~ 80 object montmorillonite particles, regrading subsequently, rinse by deionized water while screening, to be rinsed complete after, to be placed in 60 ~ 80 DEG C of baking ovens dry 6 ~ 8h, to collect to obtain 150 ~ 160 object montmorillonite particles; Count by weight, choose four oxidation three body magnetic fluid mixed liquors prepared by the montmorillonite particle of the above-mentioned preparation of 45 ~ 65 parts, the epoxy resin of 10 ~ 15 parts and 25 ~ 40 parts of steps (3), 10 ~ 15min is uniformly mixed under being placed on 600 ~ 800r/min, still aging 20 ~ 24h subsequently, it is filtered and collects filter residue, dry 6 ~ 8h in 60 ~ 80 DEG C of baking ovens, natural wind dry doubling calcination activation 2 ~ 3h at 300 ~ 400 DEG C subsequently, naturally cool to room temperature, a kind of magnetic montmorillonite Composite granule adsorbent can be prepared into.
Example 1
First 1:1 by volume, is added in the there-necked flask of 150mL by the ferric chloride solution of 0.45mol/L and the solution of ferrous chloride of 0.25mol/L, subsequently under 500r/min rotating speed, to its overtime work mixing 10min, is prepared into iron ion mixed liquor; After mixing to be mixed completes, 3:1 in mass ratio, the ammonia spirit of 1.25mol/L is added in iron ion mixed liquor, after solution blackening, to its logical nitrogen protection and to its continuation stirring 25min, subsequently to its standing separation 2min, there-necked flask is moved near magnetic field and carry out Magneto separate process 15min; Treat that solution is clarified completely, filter and collect filter residue to it, and after spending deionized water 3 times, by solid-to-liquid ratio 1:10, be dispersed in deionized water, the 25min of ultrasonic wave added vibration subsequently, is prepared into four oxidation three body magnetic fluid mixed liquors, for subsequent use; The imvite of drying is placed in high pressure milling device, to its 10min sieving of milling, be prepared into 60 object montmorillonite particles, regrading subsequently, rinse by deionized water while screening, to be rinsed complete after, be placed on dry 6h in 60 DEG C of baking ovens, collect to obtain 150 object montmorillonite particles; Count by weight, choose the montmorillonite particle of the above-mentioned preparation of 45 parts, the epoxy resin of 15 parts and 40 portions of four oxidation three body magnetic fluid mixed liquors prepared, 10min is uniformly mixed under being placed on 600r/min, still aging 20h subsequently, it is filtered and collects filter residue, dry 6h in 60 DEG C of baking ovens, subsequently natural wind dry doubling calcination activation 2h at 300 DEG C, naturally cool to room temperature, a kind of magnetic montmorillonite Composite granule adsorbent can be prepared into.
Getting magnetic montmorillonite Composite granule adsorbent that 20g obtains, to be carried on aperture be on the screen cloth of 20 μm, being holded up by screen cloth is placed in wastewater disposal basin, one is laid every 50cm, pass into the cadmium wastewater that mass concentration is 20mg/L, stop 6h, recording cadmium ion ionic adsorption capacity is 18mg/g, and adsorption rate reaches 90%.
Example 2
First 1:1 by volume, is added in the there-necked flask of 150mL by the ferric chloride solution of 0.45mol/L and the solution of ferrous chloride of 0.25mol/L, subsequently under 550r/min rotating speed, to its overtime work mixing 12min, is prepared into iron ion mixed liquor; After mixing to be mixed completes, 3:1 in mass ratio, the ammonia spirit of 1.25mol/L is added in iron ion mixed liquor, after solution blackening, to its logical nitrogen protection and to its continuation stirring 27min, subsequently to its standing separation 2 ~ 3min, there-necked flask is moved near magnetic field and carry out Magneto separate process 17min; Treat that solution is clarified completely, filter and collect filter residue to it, and after spending deionized water 4 times, by solid-to-liquid ratio 1:10, be dispersed in deionized water, the 27min of ultrasonic wave added vibration subsequently, is prepared into four oxidation three body magnetic fluid mixed liquors, for subsequent use; The imvite of drying is placed in high pressure milling device, to its 12min sieving of milling, be prepared into 70 object montmorillonite particles, regrading subsequently, rinse by deionized water while screening, to be rinsed complete after, be placed on dry 7h in 70 DEG C of baking ovens, collect to obtain 155 object montmorillonite particles; Count by weight, choose the montmorillonite particle of the above-mentioned preparation of 50 parts, the epoxy resin of 15 parts and 35 portions of four oxidation three body magnetic fluid mixed liquors prepared, 12min is uniformly mixed under being placed on 700r/min, still aging 22h subsequently, it is filtered and collects filter residue, dry 7h in 70 DEG C of baking ovens, subsequently natural wind dry doubling calcination activation 2.5h at 350 DEG C, naturally cool to room temperature, a kind of magnetic montmorillonite Composite granule adsorbent can be prepared into.
Getting magnetic montmorillonite Composite granule adsorbent that 30g obtains, to be carried on aperture be on the screen cloth of 20 μm, being holded up by screen cloth is placed in wastewater disposal basin, one is laid every 55cm, pass into the cadmium wastewater that mass concentration is 100mg/L, stop 7h, recording cadmium ion ionic adsorption capacity is 100mg/g, and adsorption rate reaches 92%.
Example 3
First 1:1 by volume, is added in the there-necked flask of 150mL by the ferric chloride solution of 0.45mol/L and the solution of ferrous chloride of 0.25mol/L, subsequently under 600r/min rotating speed, to its overtime work mixing 15min, is prepared into iron ion mixed liquor; After mixing to be mixed completes, 3:1 in mass ratio, the ammonia spirit of 1.25mol/L is added in iron ion mixed liquor, after solution blackening, to its logical nitrogen protection and to its continuation stirring 30min, subsequently to its standing separation 3min, there-necked flask is moved near magnetic field and carry out Magneto separate process 20min; Treat that solution is clarified completely, filter and collect filter residue to it, and after spending deionized water 5 times, by solid-to-liquid ratio 1:10, be dispersed in deionized water, the 30min of ultrasonic wave added vibration subsequently, is prepared into four oxidation three body magnetic fluid mixed liquors, for subsequent use; The imvite of drying is placed in high pressure milling device, to its 15min sieving of milling, be prepared into 80 object montmorillonite particles, regrading subsequently, rinse by deionized water while screening, to be rinsed complete after, be placed on dry 8h in 80 DEG C of baking ovens, collect to obtain 160 object montmorillonite particles; Count by weight, choose the montmorillonite particle of the above-mentioned preparation of 65 parts, the epoxy resin of 10 parts and 25 portions of four oxidation three body magnetic fluid mixed liquors prepared, 15min is uniformly mixed under being placed on 800r/min, still aging 24h subsequently, it is filtered and collects filter residue, dry 8h in 80 DEG C of baking ovens, subsequently natural wind dry doubling calcination activation 3h at 400 DEG C, naturally cool to room temperature, a kind of magnetic montmorillonite Composite granule adsorbent can be prepared into.
Getting magnetic montmorillonite Composite granule adsorbent that 20 ~ 40g obtains, to be carried on aperture be on the screen cloth of 20 μm, being holded up by screen cloth is placed in wastewater disposal basin, one is laid every 60cm, pass into the cadmium wastewater that mass concentration is 200mg/L, stop 8h, recording cadmium ion ionic adsorption capacity is 190mg/g, and adsorption rate reaches 93%.
Claims (1)
1. a preparation method for magnetic montmorillonite Composite granule adsorbent, is characterized in that concrete preparation process is:
(1) 1:1 by volume, the ferric chloride solution of 0.45mol/L and the solution of ferrous chloride of 0.25mol/L are added in the there-necked flask of 150mL, subsequently under 500 ~ 600r/min rotating speed, to its overtime work mixing 10 ~ 15min, be prepared into iron ion mixed liquor;
(2) after mixing to be mixed completes, 3:1 in mass ratio, the ammonia spirit of 1.25mol/L is added in iron ion mixed liquor, after solution blackening, to its logical nitrogen protection and to its continuation stirring 25 ~ 30min, subsequently to its standing separation 2 ~ 3min, there-necked flask is moved near magnetic field and carry out Magneto separate process 15 ~ 20min;
(3) treat that solution is clarified completely, it is filtered and collects filter residue, and after spending deionized water 3 ~ 5 times, by solid-to-liquid ratio 1:10, be dispersed in deionized water, the 25 ~ 30min of ultrasonic wave added vibration subsequently, be prepared into four oxidation three body magnetic fluid mixed liquors, for subsequent use;
(4) imvite of drying is placed in high pressure milling device, to its 10 ~ 15min sieving of milling, be prepared into 60 ~ 80 object montmorillonite particles, regrading subsequently, rinse by deionized water while screening, to be rinsed complete after, to be placed in 60 ~ 80 DEG C of baking ovens dry 6 ~ 8h, to collect to obtain 150 ~ 160 object montmorillonite particles;
(5) count by weight, choose four oxidation three body magnetic fluid mixed liquors prepared by the montmorillonite particle of the above-mentioned preparation of 45 ~ 65 parts, the epoxy resin of 10 ~ 15 parts and 25 ~ 40 parts of steps (3), 10 ~ 15min is uniformly mixed under being placed on 600 ~ 800r/min, still aging 20 ~ 24h subsequently, it is filtered and collects filter residue, dry 6 ~ 8h in 60 ~ 80 DEG C of baking ovens, natural wind dry doubling calcination activation 2 ~ 3h at 300 ~ 400 DEG C subsequently, naturally cool to room temperature, a kind of magnetic montmorillonite Composite granule adsorbent can be prepared into.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107081124A (en) * | 2017-04-17 | 2017-08-22 | 江苏师范大学 | In-situ preparation of montmorillonite nanoparticles and method for removing heavy metals in fruit juice by using montmorillonite nanoparticles |
| CN107189784A (en) * | 2017-06-01 | 2017-09-22 | 滨州学院 | A kind of waste old ceramics expansive soil modifier and its application method |
| CN109205729A (en) * | 2018-11-12 | 2019-01-15 | 管敏富 | Application of the mesoporous carbon adsorbent of support type in Treatment of Coking Effluent |
| CN113150393A (en) * | 2021-02-08 | 2021-07-23 | 广西春景环保科技有限公司 | Preparation method of intercalated modified montmorillonite/cassava starch composite film |
| CN113908799A (en) * | 2021-12-14 | 2022-01-11 | 山东省科学院生态研究所(山东省科学院中日友好生物技术研究中心) | Preparation method and application of magnetic Prussian blue nano clay |
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| CN101215041A (en) * | 2008-01-14 | 2008-07-09 | 中国科学院广州地球化学研究所 | Method for treating Cr6+ in waste water and method for preparing montmorillonite-base nano magnetite used thereof |
| CN102531094A (en) * | 2012-02-13 | 2012-07-04 | 扬州大学 | Treatment method of wastewater containing heavy metal ions or phosphorus |
| CN104258816A (en) * | 2014-10-24 | 2015-01-07 | 安徽工业大学 | Preparation method of magnetic stripping type montmorillonite nanocomposite material for wastewater treatment |
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2015
- 2015-12-12 CN CN201510919609.3A patent/CN105536752A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101215041A (en) * | 2008-01-14 | 2008-07-09 | 中国科学院广州地球化学研究所 | Method for treating Cr6+ in waste water and method for preparing montmorillonite-base nano magnetite used thereof |
| CN102531094A (en) * | 2012-02-13 | 2012-07-04 | 扬州大学 | Treatment method of wastewater containing heavy metal ions or phosphorus |
| CN104258816A (en) * | 2014-10-24 | 2015-01-07 | 安徽工业大学 | Preparation method of magnetic stripping type montmorillonite nanocomposite material for wastewater treatment |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107081124A (en) * | 2017-04-17 | 2017-08-22 | 江苏师范大学 | In-situ preparation of montmorillonite nanoparticles and method for removing heavy metals in fruit juice by using montmorillonite nanoparticles |
| CN107189784A (en) * | 2017-06-01 | 2017-09-22 | 滨州学院 | A kind of waste old ceramics expansive soil modifier and its application method |
| CN107189784B (en) * | 2017-06-01 | 2019-10-15 | 山东建筑大学 | A kind of waste old ceramics expansive soil modifier and its application method |
| CN109205729A (en) * | 2018-11-12 | 2019-01-15 | 管敏富 | Application of the mesoporous carbon adsorbent of support type in Treatment of Coking Effluent |
| CN109205729B (en) * | 2018-11-12 | 2021-08-06 | 管敏富 | Application of supported mesoporous carbon adsorbent in coking wastewater treatment |
| CN113150393A (en) * | 2021-02-08 | 2021-07-23 | 广西春景环保科技有限公司 | Preparation method of intercalated modified montmorillonite/cassava starch composite film |
| CN113908799A (en) * | 2021-12-14 | 2022-01-11 | 山东省科学院生态研究所(山东省科学院中日友好生物技术研究中心) | Preparation method and application of magnetic Prussian blue nano clay |
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Application publication date: 20160504 |