CN107141395A - It is a kind of for extracting resin of heavy metal-containing wastewater treatment and preparation method thereof - Google Patents

It is a kind of for extracting resin of heavy metal-containing wastewater treatment and preparation method thereof Download PDF

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Publication number
CN107141395A
CN107141395A CN201710496837.3A CN201710496837A CN107141395A CN 107141395 A CN107141395 A CN 107141395A CN 201710496837 A CN201710496837 A CN 201710496837A CN 107141395 A CN107141395 A CN 107141395A
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China
Prior art keywords
parts
resin
heavy metal
incubated
extracting
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CN201710496837.3A
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Chinese (zh)
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白才蓉
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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
    • C08F212/34Monomers containing two or more unsaturated aliphatic radicals
    • C08F212/36Divinylbenzene
    • 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
    • B01J20/26Synthetic macromolecular compounds
    • B01J20/265Synthetic macromolecular compounds modified or post-treated polymers
    • 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
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/12Polymerisation in non-solvents
    • C08F2/16Aqueous medium
    • C08F2/20Aqueous medium with the aid of macromolecular dispersing agents
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Water Supply & Treatment (AREA)
  • Environmental & Geological Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Hydrology & Water Resources (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Water Treatment By Sorption (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The present invention relates to a kind of for extracting resin of heavy metal-containing wastewater treatment and preparation method thereof, belong to resin technology field.Including oil phase:60 80 parts of divinylbenzene, 20 30 parts of styrene, 10 20 parts of hydroxyethyl methacrylate, 60 80 parts of dimethylbenzene, 40 60 parts of isooctanol, 12 parts of dibenzoyl peroxide;Aqueous phase:5 10 parts of polyvinyl alcohol, 600 800 parts of deionized water, 10 30 parts of sodium chloride, 30 50 parts of P520 phosphorus system extractant.The present invention is prepared for a kind of macroreticular resin with porous property, and fluid extractant is impregnated into inside macroreticular resin, so as to which extractant is changed into solid-state by liquid, realize the chromatographic extraction of heavy metal, both the shortcoming of liquid-liquid extraction had been overcome, the preparation technology of chelating resin is in turn simplify, product cost is reduced.Extractant species difference according to being impregnated can realize effective removal to different heavy metals.

Description

It is a kind of for extracting resin of heavy metal-containing wastewater treatment and preparation method thereof
Technical field
The present invention relates to a kind of extracting resin and preparation method thereof, it is more particularly related to which a kind of be used for containing weight Extracting resin of metallic wastewater processing and preparation method thereof, belongs to resin technology field.
Background technology
Often contain various toxic heavy metal ions in technique waste water, serious pollution is caused to environment.Especially to soil Pollution make through contaminated soil pollution recovery it is very difficult, cost is high.Therefore, develop to containing various heavy metal containing wastewater treatments A highly important research field is become with functional material.Be conventionally used to handle heavy metal-containing waste water resin have from Sub-exchange resin, chelating resin etc..Selective not high, the restricted application of the former heavy metal;The latter preparation technology is complicated, makes It is high with cost.
State Intellectual Property Office discloses a Publication No. CN102675540A, entitled " one kind weight in 2012.9.19 The invention of adsorption of metal ions resin and preparation method thereof ", the invention is specifically related to a kind of for heavy metal ion adsorbed day Right polymer modification polymeric adsorbent and preparation method thereof.A kind of Heavy metal ion adsorption resin of the present invention, its each component Weight percentage be:Chitosan (Chit) 10.0%-15.0%;Acrylic acid (AA) 25.0%-50.0%;Acrylamide (AM) 20%-45%;N, N- methylene-bisacrylamide (NMBA) 0.1%-0.4%;Potassium peroxydisulfate (KPS) 1.0%-3.0%. Wood powder also containing 0.0%-15.0% weight percentages.The Heavy metal ion adsorption resin of the present invention can efficient absorption separation Pb2+, the cost of chitin modified polymeric adsorbent is reduced, adsorption capacity and Reusability number of times is improved, improves its adsorptive selectivity. Above-mentioned resin can not handle the waste water containing heavy metal well.
The content of the invention
Present invention seek to address that the problem of resin of the prior art can not handle the waste water containing heavy metal well, carries For a kind of extracting resin for heavy metal-containing wastewater treatment, the extracting resin can effectively remove a variety of huge sum of moneys in waste water Category.
In order to realize foregoing invention purpose, its specific technical scheme is as follows:
A kind of extracting resin for heavy metal-containing wastewater treatment, it is characterised in that:Including following original in parts by weight Material:
Oil phase:
60-80 parts of divinylbenzene
20-30 parts of styrene
10-20 parts of hydroxyethyl methacrylate
60-80 parts of dimethylbenzene
40-60 parts of isooctanol
1-2 parts of dibenzoyl peroxide;
Aqueous phase:
5-10 parts of polyvinyl alcohol
600-800 parts of deionized water
10-30 parts of sodium chloride
Extractant 30-50 parts of P520 phosphorus system
A kind of preparation method of extracting resin for heavy metal-containing wastewater treatment, it is characterised in that:Comprise the following steps that:
A, according to synthesizing formula, accurately weigh polyvinyl alcohol, sodium chloride, deionized water and be put into three mouthfuls of reactors, start stirring simultaneously It is completely dissolved all components;Reaction system is heated to 65-70 DEG C;
B, oil phase component mixing is accurately weighed according to synthesizing formula, and put into three mouthfuls of reaction vessels, be warming up to 72- 75℃;Stirring, uniform bead is dispersed into by oil phase;Temperature is risen to 80 DEG C after the sizing of scattered bead, 1h is incubated;Will polymerization Temperature of reaction system is raised to 80 DEG C, is incubated 2-3h;Polymerization reaction system is warming up to 85 DEG C, 2-3h is incubated;By polymerisation body System is warming up to 90 DEG C, is incubated 2-3h;Reaction system is cooled to less than 50 DEG C, resin bead is filtered out;With originally water rinse resin, Air-dry and obtain extracting resin matrix;
C, in one have charge door, stirring and condenser pipe three mouthfuls of reaction vessels in, add and the extracting resin matrix, in room Stirring is started after the lower immersion 1h of temperature and is slowly stirred 2-3h, is filtered out resin and is produced product.
The present invention is prepared for a kind of macroreticular resin with porous property, and fluid extractant is impregnated into macroreticular resin Portion, so that extractant is changed into solid-state by liquid, realizes the chromatographic extraction of heavy metal, has both overcome lacking for liquid-liquid extraction Point, in turn simplify the preparation technology of chelating resin, reduces product cost.Extractant species difference according to being impregnated can be right Different heavy metals realize effective remove.
Embodiment
Embodiment 1
A kind of extracting resin for heavy metal-containing wastewater treatment, including following raw materials by weight:
Oil phase:
60 parts of divinylbenzene
20 parts of styrene
10 parts of hydroxyethyl methacrylate
60 parts of dimethylbenzene
40 parts of isooctanol
1 part of dibenzoyl peroxide;
Aqueous phase:
5 parts of polyvinyl alcohol
600 parts of deionized water
10 parts of sodium chloride
30 parts of P520 phosphorus system extractant.
Embodiment 2
A kind of extracting resin for heavy metal-containing wastewater treatment, including following raw materials by weight:
Oil phase:
80 parts of divinylbenzene
30 parts of styrene
20 parts of hydroxyethyl methacrylate
80 parts of dimethylbenzene
60 parts of isooctanol
2 parts of dibenzoyl peroxide;
Aqueous phase:
10 parts of polyvinyl alcohol
800 parts of deionized water
30 parts of sodium chloride
50 parts of P520 phosphorus system extractant.
Embodiment 3
A kind of extracting resin for heavy metal-containing wastewater treatment, including following raw materials by weight:
Oil phase:
70 parts of divinylbenzene
25 parts of styrene
15 parts of hydroxyethyl methacrylate
70 parts of dimethylbenzene
50 parts of isooctanol
1.5 parts of dibenzoyl peroxide;
Aqueous phase:
7.5 parts of polyvinyl alcohol
700 parts of deionized water
20 parts of sodium chloride
40 parts of P520 phosphorus system extractant.
Embodiment 4
A kind of extracting resin for heavy metal-containing wastewater treatment, including following raw materials by weight:
Oil phase:
78 parts of divinylbenzene
21 parts of styrene
13 parts of hydroxyethyl methacrylate
65 parts of dimethylbenzene
42 parts of isooctanol
1.7 parts of dibenzoyl peroxide;
Aqueous phase:
6 parts of polyvinyl alcohol
660 parts of deionized water
15 parts of sodium chloride
37 parts of P520 phosphorus system extractant.
Embodiment 5
A kind of preparation method of extracting resin for heavy metal-containing wastewater treatment, is comprised the following steps that:
A, according to synthesizing formula, accurately weigh polyvinyl alcohol, sodium chloride, deionized water and be put into three mouthfuls of reactors, start stirring simultaneously It is completely dissolved all components;Reaction system is heated to 65 DEG C;
B, oil phase component mixing is accurately weighed according to synthesizing formula, and put into three mouthfuls of reaction vessels, be warming up to 72 ℃;Stirring, uniform bead is dispersed into by oil phase;Temperature is risen to 80 DEG C after the sizing of scattered bead, 1h is incubated;It will polymerize anti- Answer system temperature to be raised to 80 DEG C, be incubated 2h;Polymerization reaction system is warming up to 85 DEG C, 2h is incubated;Polymerization reaction system is heated up To 90 DEG C, 2h is incubated;Reaction system is cooled to less than 50 DEG C, resin bead is filtered out;With originally water rinse resin, air-dry and produce To extracting resin matrix;
C, in one have charge door, stirring and condenser pipe three mouthfuls of reaction vessels in, add and the extracting resin matrix, in room Stirring is started after the lower immersion 1h of temperature and is slowly stirred 2h, is filtered out resin and is produced product.
Embodiment 6
A kind of preparation method of extracting resin for heavy metal-containing wastewater treatment, is comprised the following steps that:
A, according to synthesizing formula, accurately weigh polyvinyl alcohol, sodium chloride, deionized water and be put into three mouthfuls of reactors, start stirring simultaneously It is completely dissolved all components;Reaction system is heated to 70 DEG C;
B, oil phase component mixing is accurately weighed according to synthesizing formula, and put into three mouthfuls of reaction vessels, be warming up to 75 ℃;Stirring, uniform bead is dispersed into by oil phase;Temperature is risen to 80 DEG C after the sizing of scattered bead, 1h is incubated;It will polymerize anti- Answer system temperature to be raised to 80 DEG C, be incubated 3h;Polymerization reaction system is warming up to 85 DEG C, 3h is incubated;Polymerization reaction system is heated up To 90 DEG C, 3h is incubated;Reaction system is cooled to less than 50 DEG C, resin bead is filtered out;With originally water rinse resin, air-dry and produce To extracting resin matrix;
C, in one have charge door, stirring and condenser pipe three mouthfuls of reaction vessels in, add and the extracting resin matrix, in room Stirring is started after the lower immersion 1h of temperature and is slowly stirred 3h, is filtered out resin and is produced product.
Embodiment 7
A kind of preparation method of extracting resin for heavy metal-containing wastewater treatment, is comprised the following steps that:
A, according to synthesizing formula, accurately weigh polyvinyl alcohol, sodium chloride, deionized water and be put into three mouthfuls of reactors, start stirring simultaneously It is completely dissolved all components;Reaction system is heated to 67.5 DEG C;
B, oil phase component mixing is accurately weighed according to synthesizing formula, and put into three mouthfuls of reaction vessels, is warming up to 73.5℃;Stirring, uniform bead is dispersed into by oil phase;Temperature is risen to 80 DEG C after the sizing of scattered bead, 1h is incubated;Will be poly- Close temperature of reaction system and be raised to 80 DEG C, be incubated 2.5h;Polymerization reaction system is warming up to 85 DEG C, 2.5h is incubated;By polymerisation System is warming up to 90 DEG C, is incubated 2.5h;Reaction system is cooled to less than 50 DEG C, resin bead is filtered out;Rinsed and set with running water Fat, air-dries and obtains extracting resin matrix;
C, in one have charge door, stirring and condenser pipe three mouthfuls of reaction vessels in, add and the extracting resin matrix, in room Stirring is started after the lower immersion 1h of temperature and is slowly stirred 2.5h, is filtered out resin and is produced product.
Embodiment 8
A kind of preparation method of extracting resin for heavy metal-containing wastewater treatment, is comprised the following steps that:
A, according to synthesizing formula, accurately weigh polyvinyl alcohol, sodium chloride, deionized water and be put into three mouthfuls of reactors, start stirring simultaneously It is completely dissolved all components;Reaction system is heated to 66 DEG C;
B, oil phase component mixing is accurately weighed according to synthesizing formula, and put into three mouthfuls of reaction vessels, be warming up to 73 ℃;Stirring, uniform bead is dispersed into by oil phase;Temperature is risen to 80 DEG C after the sizing of scattered bead, 1h is incubated;It will polymerize anti- Answer system temperature to be raised to 80 DEG C, be incubated 2.6h;Polymerization reaction system is warming up to 85 DEG C, 2.9h is incubated;By polymerization reaction system 90 DEG C are warming up to, 2.25h is incubated;Reaction system is cooled to less than 50 DEG C, resin bead is filtered out;With originally water rinse resin, Air-dry and obtain extracting resin matrix;
C, in one have charge door, stirring and condenser pipe three mouthfuls of reaction vessels in, add and the extracting resin matrix, in room Stirring is started after the lower immersion 1h of temperature and is slowly stirred 2.6h, is filtered out resin and is produced product.

Claims (2)

1. a kind of extracting resin for heavy metal-containing wastewater treatment, it is characterised in that:Including it is following in parts by weight Raw material:
Oil phase:
60-80 parts of divinylbenzene
20-30 parts of styrene
10-20 parts of hydroxyethyl methacrylate
60-80 parts of dimethylbenzene
40-60 parts of isooctanol
1-2 parts of dibenzoyl peroxide;
Aqueous phase:
5-10 parts of polyvinyl alcohol
600-800 parts of deionized water
10-30 parts of sodium chloride
Extractant 30-50 parts of P520 phosphorus system.
2. a kind of preparation method of extracting resin for heavy metal-containing wastewater treatment, it is characterised in that:Including following technique step Suddenly:
A, according to synthesizing formula, accurately weigh polyvinyl alcohol, sodium chloride, deionized water and be put into three mouthfuls of reactors, start stirring simultaneously It is completely dissolved all components;Reaction system is heated to 65-70 DEG C;
B, oil phase component mixing is accurately weighed according to synthesizing formula, and put into three mouthfuls of reaction vessels, be warming up to 72- 75℃;Stirring, uniform bead is dispersed into by oil phase;Temperature is risen to 80 DEG C after the sizing of scattered bead, 1h is incubated;Will polymerization Temperature of reaction system is raised to 80 DEG C, is incubated 2-3h;Polymerization reaction system is warming up to 85 DEG C, 2-3h is incubated;By polymerisation body System is warming up to 90 DEG C, is incubated 2-3h;Reaction system is cooled to less than 50 DEG C, resin bead is filtered out;With originally water rinse resin, Air-dry and obtain extracting resin matrix;
C, in one have charge door, stirring and condenser pipe three mouthfuls of reaction vessels in, add and the extracting resin matrix, in room Stirring is started after the lower immersion 1h of temperature and is slowly stirred 2-3h, is filtered out resin and is produced product.
CN201710496837.3A 2017-06-27 2017-06-27 It is a kind of for extracting resin of heavy metal-containing wastewater treatment and preparation method thereof Pending CN107141395A (en)

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CN201710496837.3A CN107141395A (en) 2017-06-27 2017-06-27 It is a kind of for extracting resin of heavy metal-containing wastewater treatment and preparation method thereof

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CN201710496837.3A CN107141395A (en) 2017-06-27 2017-06-27 It is a kind of for extracting resin of heavy metal-containing wastewater treatment and preparation method thereof

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20040055217A (en) * 2002-12-20 2004-06-26 한국지질자원연구원 A method for manufacturing extraction rosin for extraction and separation of an rare earth element
CN101139418A (en) * 2007-07-19 2008-03-12 四川大学 Elution-extracting resin using amide compound as extracting agent and preparation method thereof
CN103691146A (en) * 2013-12-09 2014-04-02 何小刚 Extraction agent of impregnating resin and preparation method thereof
CN106317284A (en) * 2016-08-12 2017-01-11 辽宁大学 Extraction-elution resin chelated with P507 extraction agent and preparation method and application of extraction-elution resin

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20040055217A (en) * 2002-12-20 2004-06-26 한국지질자원연구원 A method for manufacturing extraction rosin for extraction and separation of an rare earth element
CN101139418A (en) * 2007-07-19 2008-03-12 四川大学 Elution-extracting resin using amide compound as extracting agent and preparation method thereof
CN103691146A (en) * 2013-12-09 2014-04-02 何小刚 Extraction agent of impregnating resin and preparation method thereof
CN106317284A (en) * 2016-08-12 2017-01-11 辽宁大学 Extraction-elution resin chelated with P507 extraction agent and preparation method and application of extraction-elution resin

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
PARK, JS等: "Synthesis of extraction resin containing 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester and its performance for separation of rare earths (Gd, Tb)", 《SEPARATION AND PURIFICATION TECHNOLOGY》 *

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