CN107325215A - It is a kind of for high molecule magnetic microsphere of phenol in wastewater adsorption treatment and preparation method thereof - Google Patents

It is a kind of for high molecule magnetic microsphere of phenol in wastewater adsorption treatment and preparation method thereof Download PDF

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Publication number
CN107325215A
CN107325215A CN201710496842.4A CN201710496842A CN107325215A CN 107325215 A CN107325215 A CN 107325215A CN 201710496842 A CN201710496842 A CN 201710496842A CN 107325215 A CN107325215 A CN 107325215A
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parts
phenol
high molecule
magnetic
magnetic microsphere
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CN201710496842.4A
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彭雅龙
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F212/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
    • C08F212/02Monomers containing only one unsaturated aliphatic radical
    • C08F212/04Monomers containing only one unsaturated aliphatic radical containing one ring
    • C08F212/06Hydrocarbons
    • C08F212/08Styrene
    • 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
    • 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
    • B01J20/28014Solid 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 form
    • B01J20/28016Particle form
    • B01J20/28021Hollow particles, e.g. hollow spheres, microspheres or cenospheres
    • 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
    • C02F1/285Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • C02F2101/345Phenols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2265Oxides; Hydroxides of metals of iron
    • C08K2003/2275Ferroso-ferric oxide (Fe3O4)

Abstract

The present invention relates to a kind of for high molecule magnetic microsphere of phenol in wastewater adsorption treatment and preparation method thereof, belong to high molecule magnetic microsphere technical field.Including oil phase:35 parts of styrene, 20 parts of methyl methacrylate, 15 parts of divinylbenzene, 5 parts of azodiisobutyronitrile, 15 parts of magnetic fluid;Aqueous phase:10 parts of polyvinyl alcohol, 3 parts of gelatin, 20 parts of sodium chloride, 500 parts of deionized water.Obtained high molecule magnetic microsphere uniform particle sizes, magnetic responsiveness is strong, can be efficiently applied to the processing of wastewater containing phenol.Have broad application prospects.

Description

A kind of high molecule magnetic microsphere and its preparation for phenol in wastewater adsorption treatment Method
Technical field
The present invention relates to a kind of high molecule magnetic microsphere and preparation method thereof, it is more particularly related to which a kind of use In high molecule magnetic microsphere of phenol in wastewater adsorption treatment and preparation method thereof, belong to high molecule magnetic microsphere technical field.
Background technology
High molecule magnetic microsphere is a kind of new function material that developed recently gets up.Containing a magnetic core inside microballoon, Therefore, in the presence of external magnetic field, microballoon can be separated easily with bottom liquid;Meanwhile, the macromolecule layer surface of microballoon can be repaiied Various active group is adornd, enables microballoon further functionalization, connects various chemical groups and be widely used in and cell, enzyme, albumen The biological substances such as matter, antibody, nucleic acid are coupled and the various processing containing toxic organic compound waste water.In post processing(Desorption, regeneration Deng)Stage can realize that material is separated with waste water under magnetic fields, and its operating process is easy, and separative efficiency is much better than conventional separation Method.Therefore, magnetic microsphere is widely used in biochemistry.At present, the preparation method of magnetic microsphere mainly has embedding Method, suspension polymerization, infusion process and biological synthesis process(Jing Xiaoyan, Li Rumin, Wang Peng etc., analytical chemistry, 1999,27 (12): 1462—1467;Qiu Guangming, Sun Zonghua, chemical reagent, 1993,15 (4):234-237,255;Zhang Shenglong, Peng Tuzhi, Yang C.F.J.Electroana1.Chem., 2002,522 (2):152—157;Qiu Guangming, Gao Xiaosong, poplar Spring wild goose, applied chemistry, 1996,13 (1):6 9).Compared with other method for preparing microsphere, suspension polymerization has significant excellent Point.The method can efficiently control the particle size range of microballoon.And the species of microsphere surface active group can be controlled.Therefore use and suspend Polymerization prepares magnetic microsphere and extremely paid attention to.Existing high molecule magnetic microsphere can not handle the benzene in absorption waste water well Phenol.
The content of the invention
Present invention seek to address that high molecule magnetic microsphere can not handle absorption phenol in wastewater well in the prior art Problem is there is provided a kind of high molecule magnetic microsphere for phenol in wastewater adsorption treatment, and the magnetic microsphere particle diameter is uniform, magnetic response Property it is strong, the processing of wastewater containing phenol can be efficiently applied to.
In order to realize foregoing invention purpose, its specific technical scheme is as follows:
A kind of high molecule magnetic microsphere for phenol in wastewater adsorption treatment, it is characterised in that:Including below according to parts by weight The raw material of number meter:
Oil phase:
35 parts of styrene
20 parts of methyl methacrylate
15 parts of divinylbenzene
5 parts of azodiisobutyronitrile
15 parts of magnetic fluid;
Aqueous phase:
10 parts of polyvinyl alcohol
3 parts of gelatin
20 parts of sodium chloride
500 parts of deionized water.
A kind of preparation method of high molecule magnetic microsphere for phenol in wastewater adsorption treatment, it is characterised in that:Including Following processing step:
A, according to recipe requirements, prepare aqueous phase;With ultrasonoscope ultrasonic disperse 10-15min;It is sequentially added under nitrogen protection pre- The oil phase first prepared;
B, start mechanical agitation and disperse 10-15min, and reaction temperature is risen to 70-75 DEG C;Mixing speed is controlled in 200- 2h is reacted at 250r/min, 75-80 DEG C;2h is reacted at 80-85 DEG C;5h is reacted at 85-90 DEG C;
C, reaction temperature is down to room temperature, Magnetic filter goes out hard resin, uses absolute ethyl alcohol cyclic washing, obtains High Polymer Magnetic micro- Ball.
The high molecule magnetic microsphere prepared with above-mentioned technique between 40-50mg/ml, is passed through to the adsorbance of phenol in wastewater After zeolite regeneration can Reusability, effective usage cycles be 100 or so.
The advantageous effects that the present invention is brought:
The present invention uses suspended dispersed polymerization, in magnetic fluid Fe2O3In the presence of, using water as decentralized medium, with polyvinyl alcohol alcohol For dispersant and stabilizer, reaction solution is pre-processed using ultrasonic wave, makes magnetic fluid Fe2O3Polymerization can be preferably dispersed in In reaction solution.Meanwhile, enable the copolyreaction of styrene and acrylic acid in Fe2O3Magnetic-particle surface is smoothed out.It is made The high molecule magnetic microsphere uniform particle sizes obtained, magnetic responsiveness is strong, can be efficiently applied to the processing of wastewater containing phenol.With wide Application prospect.
Embodiment
Embodiment 1
A kind of high molecule magnetic microsphere for phenol in wastewater adsorption treatment, including following raw materials by weight:
Oil phase:
35 parts of styrene
20 parts of methyl methacrylate
15 parts of divinylbenzene
5 parts of azodiisobutyronitrile
15 parts of magnetic fluid;
Aqueous phase:
10 parts of polyvinyl alcohol
3 parts of gelatin
20 parts of sodium chloride
500 parts of deionized water.
Embodiment 2
A kind of preparation method of high molecule magnetic microsphere for phenol in wastewater adsorption treatment, is comprised the following steps that:
A, according to recipe requirements, prepare aqueous phase;With ultrasonoscope ultrasonic disperse 10min;It is sequentially added under nitrogen protection in advance The oil phase prepared;
B, start mechanical agitation and disperse 10min, and reaction temperature is risen to 70 DEG C;Mixing speed is controlled in 200r/min, 75 2h is reacted at DEG C;2h is reacted at 80 DEG C;5h is reacted at 85 DEG C;
C, reaction temperature is down to room temperature, Magnetic filter goes out hard resin, uses absolute ethyl alcohol cyclic washing, obtains High Polymer Magnetic micro- Ball.
Embodiment 3
A kind of preparation method of high molecule magnetic microsphere for phenol in wastewater adsorption treatment, is comprised the following steps that:
A, according to recipe requirements, prepare aqueous phase;With ultrasonoscope ultrasonic disperse 15min;It is sequentially added under nitrogen protection in advance The oil phase prepared;
B, start mechanical agitation and disperse 15min, and reaction temperature is risen to 75 DEG C;Mixing speed is controlled in 250r/min, 80 2h is reacted at DEG C;2h is reacted at 85 DEG C;5h is reacted at 90 DEG C;
C, reaction temperature is down to room temperature, Magnetic filter goes out hard resin, uses absolute ethyl alcohol cyclic washing, obtains High Polymer Magnetic micro- Ball.
Embodiment 4
A kind of preparation method of high molecule magnetic microsphere for phenol in wastewater adsorption treatment, is comprised the following steps that:
A, according to recipe requirements, prepare aqueous phase;With ultrasonoscope ultrasonic disperse 12.5min;It is sequentially added under nitrogen protection pre- The oil phase first prepared;
B, start mechanical agitation and disperse 12.5min, and reaction temperature is risen to 72.5 DEG C;Mixing speed is controlled in 225r/ Min, reacts 2h at 77.5 DEG C;2h is reacted at 82.5 DEG C;5h is reacted at 87.5 DEG C;
C, reaction temperature is down to room temperature, Magnetic filter goes out hard resin, uses absolute ethyl alcohol cyclic washing, obtains High Polymer Magnetic micro- Ball.
Embodiment 5
A kind of preparation method of high molecule magnetic microsphere for phenol in wastewater adsorption treatment, is comprised the following steps that:
A, according to recipe requirements, prepare aqueous phase;With ultrasonoscope ultrasonic disperse 11min;It is sequentially added under nitrogen protection in advance The oil phase prepared;
B, start mechanical agitation and disperse 12min, and reaction temperature is risen to 73 DEG C;Mixing speed is controlled in 211r/min, 76 2h is reacted at DEG C;2h is reacted at 82 DEG C;5h is reacted at 88 DEG C;
C, reaction temperature is down to room temperature, Magnetic filter goes out hard resin, uses absolute ethyl alcohol cyclic washing, obtains High Polymer Magnetic micro- Ball.

Claims (2)

1. a kind of high molecule magnetic microsphere for phenol in wastewater adsorption treatment, it is characterised in that:Including below according to weight The raw material of number meter:
Oil phase:
35 parts of styrene
20 parts of methyl methacrylate
15 parts of divinylbenzene
5 parts of azodiisobutyronitrile
15 parts of magnetic fluid;
Aqueous phase:
10 parts of polyvinyl alcohol
3 parts of gelatin
20 parts of sodium chloride
500 parts of deionized water.
2. a kind of preparation side of high molecule magnetic microsphere for phenol in wastewater adsorption treatment according to claim 1 Method, it is characterised in that:Comprise the following steps that:
A, according to recipe requirements, prepare aqueous phase;With ultrasonoscope ultrasonic disperse 10-15min;It is sequentially added under nitrogen protection pre- The oil phase first prepared;
B, start mechanical agitation and disperse 10-15min, and reaction temperature is risen to 70-75 DEG C;Mixing speed is controlled in 200- 2h is reacted at 250r/min, 75-80 DEG C;2h is reacted at 80-85 DEG C;5h is reacted at 85-90 DEG C;
C, reaction temperature is down to room temperature, Magnetic filter goes out hard resin, uses absolute ethyl alcohol cyclic washing, obtains High Polymer Magnetic micro- Ball.
CN201710496842.4A 2017-06-27 2017-06-27 It is a kind of for high molecule magnetic microsphere of phenol in wastewater adsorption treatment and preparation method thereof Pending CN107325215A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115646457A (en) * 2022-10-21 2023-01-31 厦门百霖净水科技有限公司 Heavy metal removing additive, heavy metal removing carbon rod and preparation method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1053622A (en) * 1991-01-29 1991-08-07 华南理工大学 Preparation of magnetic macroporous ion-exchange resin for adsorption
CN103739764A (en) * 2013-12-09 2014-04-23 何小刚 Magnetic macroporous adsorption resin microspheres, and preparation method thereof
CN104072656A (en) * 2014-05-19 2014-10-01 河北科技大学 Method for preparing ferroferric oxide-macromolecule magnetic composite microspheres

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1053622A (en) * 1991-01-29 1991-08-07 华南理工大学 Preparation of magnetic macroporous ion-exchange resin for adsorption
CN103739764A (en) * 2013-12-09 2014-04-23 何小刚 Magnetic macroporous adsorption resin microspheres, and preparation method thereof
CN104072656A (en) * 2014-05-19 2014-10-01 河北科技大学 Method for preparing ferroferric oxide-macromolecule magnetic composite microspheres

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115646457A (en) * 2022-10-21 2023-01-31 厦门百霖净水科技有限公司 Heavy metal removing additive, heavy metal removing carbon rod and preparation method
CN115646457B (en) * 2022-10-21 2024-03-15 厦门百霖净水科技有限公司 Heavy metal removing additive, heavy metal removing carbon rod and preparation method

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Application publication date: 20171107