CN108371946A - A kind of application by bisphenol-A and the preparation method and its absorbing heavy metal ions in water of the rich nitride polyporous material of melamine polycondensation - Google Patents
A kind of application by bisphenol-A and the preparation method and its absorbing heavy metal ions in water of the rich nitride polyporous material of melamine polycondensation Download PDFInfo
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- CN108371946A CN108371946A CN201810433655.6A CN201810433655A CN108371946A CN 108371946 A CN108371946 A CN 108371946A CN 201810433655 A CN201810433655 A CN 201810433655A CN 108371946 A CN108371946 A CN 108371946A
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- bisphenol
- heavy metal
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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 present invention relates to a kind of applications by bisphenol-A and the preparation method and its absorbing heavy metal ions in water of the rich nitride polyporous material of melamine polycondensation, bisphenol-A will be copolymerized with melamine in alkaline solution, generate canescence porous material PBPAM, using the heavy metal ion in the porous material absorption sewage, achieve the purpose that purify sewage.The present invention provides a kind of efficient heavy metal ion adsorbing material PBPAM, the organic porous material can adsorbing heavy metal ions in sewage, porous material is reusable, greatly saves cost, reduces discharge of wastewater, generates economical and environmentally friendly benefit.
Description
Technical field
The present invention relates to the applications in a kind of preparation method of novel porous materials and its sewage disposal, and in particular to a kind of
The preparation method of rich nitride polyporous material made of bisphenol-A and melamine polycondensation and its use the porous material absorption heavy metal
Ion removes the application of heavy metal ions in sewage.
Background technology
Heavy metal refers to the metallic element that atomic mass is between 63.5 and 200.6 or density is 4.0 or 5.0 or more.
It includes mainly the heavy metal for having notable toxicity to biology, such as chromium, mercury, zinc, lead and micro- toxic heavy metal, as copper,
Environmental pollution caused by zinc, cobalt, cadmium etc..In addition, although selenium, arsenic are nonmetallic, but its chemical property and toxicity and a huge sum of money
Symbolic animal of the birth year seemingly, so being also put within the scope of heavy metal contaminants.
Heavy metal pollution has the characteristics that type is various, not degradable, migration is poor, irreversibility and chronicity.With much money
Belong to after entering environment, chemical property is metastable.Then, plurality of heavy metal will be constantly enriched with after entering environment.
With the increase of heavy metal concentration in environment, the toxicity of heavy metal is increasingly apparent, to influence biological nature in environment and
The structure of microbiologic population, eventually in welding ecologic structure and function stability.
Administering the common methods of heavy metal pollution and technology at present mainly has：Electrochemical process, the precipitation method, ion-exchange,
Membrane separation technique, absorption method etc..These technology and methods have its respective application characteristic.
Electrochemical method is one of the common methods of heavy metal ion handled in waste water.Electrochemistry is mainly former using electrolysis
Reason, make heavy metal ion that redox reaction occur respectively on two electrodes in waste water, make heavy metal accumulation on the electrode with
Achieve the purpose that recycle heavy metal.Currently, electrochemical method processing waste water has been widely applied in actual production.
Chemical precipitation method is a kind of more traditional method for treating water.According to the difference of type of precipitation, it is broadly divided into neutralization
The precipitation method, sulphide precipitation and ferrite process.Its principle is mainly by inside input alkali, sulfide or molysite and waste water
Metal cation act on forming hydroxide precipitation, sulfide precipitation or complex ferrite, then carry out separation of solid and liquid operation, from
And achieve the effect that heavy-metal ion removal.
It is mainly to be carried out using the metal ion in ion exchange resin, with waste water that ion-exchange, which handles heavy metal ion,
A kind of separation method exchanged.Most common cation-exchanger is the sulfonic group (- SO of highly acidic resin3) and weak acid resin H
Carboxylic acid group (- COOH).Hydrogen ion on the resin for obtaining carboxylic acid group containing sulfonic group can be swapped with metal cation,
Metal ion in this way in solution is just exchanged.The major advantage of ion-exchange has：Synthetic method is simple, performance is stable, hands over
Change that capacity is big, renewable, favorable repeatability.But ion exchange resin it is similar to like charges ion or physico-chemical property from
The poor selectivity of son, regeneration are difficult.
Membrane separation technique is to handle a kind of new method of heavy metal ion.It mainly uses permselectivity membrane,
Make the solute in solution and solute separation under certain external driving force effect, to achieve the purpose that purification, concentration and purification.
Absorption method is currently generally acknowledged processing heavy metal in waste water method the most cost-effective.Absorption method not only operates letter
Single, flexible design, and the process adsorbed often is reversible, can after wastewater treatment using suitable reagent to material into
Row parsing is reused.In absorption method, the selection of adsorbent is most important link.The property of adsorbent directly affects a huge sum of money
Belong to the separation and enrichment of ion.General adsorbent usually has following features at present：Pore structure appropriate, larger specific surface area and
Suitable surface texture has adsorbate stronger adsorption capacity, usually chemical reaction, manufacture does not occur with adsorbate or medium
Simply, regeneration etc. after parsing can be passed through.
Currently, having many kinds of substance is used as sorbing material, such as：Activated carbon, molecular sieve, chelate sorbent, is received zeolite
Rice material metal Porous-Organic framework material, organic porous polymer material etc..Kavand etc. is utilized and is extracted from useless olivine
Activated carbon Study on adsorption properties has been made to metal ions such as heavy metal lead, cadmium, nickel in water as sorbing material, obtain：It should
Kind activated carbon is to Pb2+、Ni2+、Ni2+All there is good adsorption effect.At room temperature with carbon nanotube to the Cu in water2+、Zn2 +、Pb2+、Cd2+、Co2+It is adsorbed, finally obtains the material to Pb2+Adsorption effect it is best.Research is found：In molecular structure
Contain-NH2,-NH, the groups such as-CN material better absorption property is shown to heavy metal ion.Therefore, R and D
The novel porous adsorbing material containing more nitrogen systems is significant.
Organic porous polymer (Porous Organic Frameworks, POFs) material is a kind of light by C, H, O, N etc.
The novel nano-material with abundant pore structure of prime element composition.Compared with traditional zeolitic material, it has apparent
Advantage：Light, high-specific surface area, controllable pore passage structure.With metal organic framework (Metal more popular in recent years
Organic Frameworks, MOFs) material compares, and molecule is mainly formed by covalent bond, therefore material has more stability,
It is not easy to cave in.
Organic porous polymer has been widely used in heavy metal ion adsorbed field.The study found that Porous-Organic
Material is to the heavy metal ion Hg in water2+、Cu2+、Cd2+、Ni2+、Zn2+And Co2+Deng all with higher removal rate.
Invention content
Present invention method easy to use, uses cheap common industrial goods bisphenol-A (BPA) and melamine
(Melamine) polycondensation prepares a kind of organic porous material PBPAM, and heavy metal ion is adsorbed with it, purifies sewage, a recycling huge sum of money
Belong to salt recycling, realization is turned waste into wealth, and the target of sewage discharge is reduced.Therefore, meet environmental protection and green environment requirement.It can be pre-
Phase, the material can on a large scale be applied in industrialized production from now on.
To achieve the above object, technical solution provided by the invention is：
A kind of rich nitride polyporous material by bisphenol-A and melamine polycondensation, will be to bisphenol-A and melamine in alkaline solution
Middle copolymerization generates canescence porous material PBPAM；Its specific preparation process is：Using ethylene glycol as solvent, be added melamine and
Bisphenol-A carries out heating polycondensation, is eventually adding dimethylbenzene dehydration.
Answering for heavy metal ion of the prepared rich nitride polyporous material PBPAM in absorption effluent is also disclosed in the present invention
With.
Using the heavy metal ion in the porous material absorption sewage, achieve the purpose that purify sewage, steps are as follows；
Step 1. ethylene glycol is solvent, and melamine and bisphenol-A is added, and heating polycondensation obtains porous material PBPAM.
Porous material is packed into adsorption column by step 2., will contain heavy metal ion sewage and adsorption column, adsorption column absorption is added
Heavy metal ion.
1% diluted hydrochloric acid aqueous solution is washed adsorption column, heavy metal ion desorption by step 3..
Wherein：In step 1, the molar ratio of melamine and bisphenol-A is 3:1.8~2.4；Molar ratio is less than 3：1.8 or big
In 3：When 2.4, yield is substantially reduced, and material physical property reduces.It is 8~15 hours to heat the polycondensation time, and the time is less than 8
Hour, reaction yield reduces, and yield is more than 15 hours, and yield does not significantly improve.Heating temperature is 150~198 DEG C, and temperature is low
When 150 DEG C, the reaction time is elongated, and ethylene glycol boiling point is 198 DEG C；It is eventually adding dimethylbenzene to be dehydrated 3-5 hours, the time is less than 3
Hour polycondensation is incomplete, low yield, is more than 5 hours, does not significantly improve.Dehydration temperaturre is 136-140 DEG C of xylene boiling point.
In step 2, sorbing material is 15~20 with heavy metal mass ratio in sewage：1, ratio is less than 15：When 1, absorption
Not exclusively；Ratio is more than 20：When 1, remaining precious metal concentration is not substantially reduced.
In step 3, desorption terminal is judged using atomic absorption spectrum.
Compared with prior art, the beneficial effects of the invention are as follows：
The absorption of heavy metal ions in sewage can reduce pollution, provide valuable raw material, environmental protection.The present invention provides
A kind of efficient heavy metal ion adsorbing material PBPAM, the organic porous material can adsorbing heavy metal ions in sewage, it is porous
Material is reusable, greatly saves cost, reduces discharge of wastewater, generates economical and environmentally friendly benefit.
Description of the drawings
Fig. 1：Material PBPAM preparation routes of the present invention and Adsorption and desorption heavy metal ion schematic diagram.
Fig. 2：The infrared spectrum of PBPAM, bisphenol-A and melamine (B).
Specific implementation mode
The present invention is further explained in the light of specific embodiments.
The synthesis of material：
Embodiment 1.
In 1L ethylene glycol, the melamine of 0.20mol and the bisphenol-A of 0.30mol is added, heats, stirring keeps temperature
Stabilization is reacted 10 hours at 180 DEG C, and 300mL dimethylbenzene is added, loads onto water knockout drum, and 136-140 DEG C of refluxing xylene takes away moisture,
Polycondensation 4 hours stops stirring, and Temperature fall to room temperature filters gray precipitate, and 100mL hot water washs three times；100mL ethyl alcohol is washed
It washs three times, 80 DEG C of vacuum drying obtain pale powder 72.7g yields 87.7%.
Embodiment 2.
In 1L ethylene glycol, the melamine of 0.18mol and the bisphenol-A of 0.30mol is added, heats, stirring keeps temperature
Stabilization is reacted 10 hours at 180 DEG C, and 300mL dimethylbenzene is added, loads onto water knockout drum, and 136-140 DEG C of refluxing xylene takes away moisture,
Polycondensation 4 hours stops stirring, and Temperature fall to room temperature filters to obtain gray precipitate, and 100mL hot water washs three times；100mL ethyl alcohol
Three times, 80 DEG C of vacuum drying obtain pale solid 65.4g yields 87.7% for washing.
Embodiment 3.
In 1L ethylene glycol, the melamine of 0.24mol and the bisphenol-A of 0.30mol is added, heats, stirring keeps temperature
Stabilization is reacted 10 hours at 180 DEG C, and 300mL dimethylbenzene is added, loads onto water knockout drum, and 136-140 DEG C of refluxing xylene takes away moisture,
Polycondensation 4 hours stops stirring, and Temperature fall to room temperature filters to obtain gray precipitate, and 100mL hot water washs three times；100mL ethyl alcohol
Three times, 80 DEG C of vacuum drying obtain pale solid 70.4g yields 84.9% for washing.
From embodiment 1-3 it is found that when the molar ratio of melamine and bisphenol-A is 1.8~2.4:When 3, reaction yield is higher.
To be 2 according to the molar ratio of melamine and bisphenol-A:3, it is expanded on further in embodiment.
Embodiment 4.
In 1L ethylene glycol, the melamine of 0.20mol and the bisphenol-A of 0.30mol is added, heats, stirring keeps temperature
Stabilization is reacted 10 hours at 150 DEG C, and 300mL dimethylbenzene is added, loads onto water knockout drum, and 136-140 DEG C of refluxing xylene takes away moisture,
Polycondensation 4 hours stops stirring, and Temperature fall to room temperature filters to obtain gray precipitate, and 100mL hot water washs three times；100mL ethyl alcohol
Three times, 80 DEG C of vacuum drying obtain pale solid 67.2g yields 81.1% for washing.
Embodiment 5.
In 1L ethylene glycol, the melamine of 0.20mol and the bisphenol-A of 0.30mol is added, heats, stirring keeps temperature
Stabilization is reacted 10 hours at 198 DEG C, and 300mL dimethylbenzene is added, loads onto water knockout drum, and 136-140 DEG C of refluxing xylene takes away moisture,
Polycondensation 4 hours stops stirring, and Temperature fall to room temperature filters to obtain gray precipitate, and 100mL ethyl alcohol washs three times, and 80 DEG C of vacuum are dry
It is dry, obtain pale solid 73.4g yields 88.5%.
From embodiment 1,4,5 it is found that when reaction temperature is at 150~198 DEG C, reaction yield is stablized.Will according to 180 DEG C
It is expanded on further in embodiment.
Embodiment 6.
In 1L ethylene glycol, the melamine of 0.20mol and the bisphenol-A of 0.30mol is added, heats, stirring keeps temperature
Stabilization is reacted 15 hours at 180 DEG C, and 300mL dimethylbenzene is added, loads onto water knockout drum, and 136-140 DEG C of refluxing xylene takes away moisture,
Polycondensation 4 hours stops stirring, and Temperature fall to room temperature filters to obtain gray precipitate, and 100mL hot water washs three times；100mL ethyl alcohol
Three times, 80 DEG C of vacuum drying obtain pale solid 73.0g yields 88.0% for washing.
Embodiment 7.
In 1L ethylene glycol, the melamine of 0.20mol and the bisphenol-A of 0.30mol is added, heats, stirring keeps temperature
Stabilization is reacted 8 hours at 180 DEG C, and 300mL dimethylbenzene is added, loads onto water knockout drum, and 136-140 DEG C of refluxing xylene takes away moisture,
Polycondensation 4 hours stops stirring, and Temperature fall to room temperature filters to obtain gray precipitate, and 100mL hot water washs three times；100mL ethyl alcohol
Three times, 80 DEG C of vacuum drying obtain pale solid 68.9g yields 83.1% for washing.
From embodiment 1,6,7 it is found that at 8-15 hours between when reacted, reaction yield is stablized.It will be according to 10 hours in reality
It applies in example and is expanded on further.
Embodiment 8.
In 1L ethylene glycol, the melamine of 0.20mol and the bisphenol-A of 0.30mol is added, heats, stirring keeps temperature
Stabilization is reacted 10 hours at 180 DEG C, and 300mL dimethylbenzene is added, loads onto water knockout drum, and 136-140 DEG C of refluxing xylene takes away moisture,
Polycondensation 3 hours stops stirring, and Temperature fall to room temperature filters to obtain gray precipitate, and 100mL hot water washs three times；100mL ethyl alcohol
Three times, 80 DEG C of vacuum drying obtain pale solid 70.3g yields 84.8% for washing.
Embodiment 9.
In 1L ethylene glycol, the melamine of 0.20mol and the bisphenol-A of 0.30mol is added, heats, stirring keeps temperature
Stabilization is reacted 10 hours at 180 DEG C, and 300mL dimethylbenzene is added, loads onto water knockout drum, and 136-140 DEG C of refluxing xylene takes away moisture,
Polycondensation 5 hours stops stirring, and Temperature fall to room temperature filters to obtain gray precipitate, and 100mL hot water washs three times；100mL ethyl alcohol
Three times, 80 DEG C of vacuum drying obtain pale solid 73.3g yields 88.4% for washing.
The property experiment of material：
Embodiment 10.
Above-mentioned porous material 4g is taken, is added in the aqueous solution for containing copper ion 800ppm, pH=5.5 containing 3L, room temperature is stirred
30min is mixed, is filtered, Atomic Absorption Spectrometry residue copper ion concentration is 15.3ppm, adsorption rate 98.1%.
The material for adsorbing copper ion is packed into adsorption column, is eluted using the hydrochloric acid solution of 1wt%, Atomic Absorption Spectrometry
It flows out when copper ion concentration in hydrochloric acid solution is less than 2ppm and stops elution, spend hydrochloric acid 63.5mL.
Embodiment 11.
Above-mentioned porous material 4g is taken, is added in the aqueous solution for containing zinc ion 800ppm, pH=5.5 containing 3L, room temperature is stirred
30min is mixed, is filtered, Atomic Absorption Spectrometry residue concentration of silver ions is 17.2ppm, adsorption rate 97.9%.
The material for adsorbing zinc is packed into adsorption column, is eluted using the hydrochloric acid solution of 1wt%, Atomic Absorption Spectrometry outflow
Stop elution when zinc ion concentration is less than 2ppm in hydrochloric acid solution, spends hydrochloric acid 54.6mL.
Embodiment 12.
Above-mentioned porous material 4g is taken, is added in the aqueous solution for containing lead ion 800ppm, pH=5.5 containing 3L, room temperature is stirred
30min is mixed, is filtered, Atomic Absorption Spectrometry residue plumbum ion concentration is respectively 10.1ppm, and adsorption rate is respectively 98.7%.
The material of Adsorption of Lead metal ion is packed into adsorption column, is eluted with the salpeter solution of 1wt%, atomic absorption spectrum is surveyed
Stop elution when constant current goes out lead metal ion concentration less than 2ppm, spends nitric acid 30.6mL.
The above is only presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, any ripe
Professional and technical personnel is known, without departing from the scope of the present invention, according to the technical essence of the invention, to above real
Apply any simple modification, equivalent replacement and improvement etc. made by example, still fall within technical solution of the present invention protection domain it
It is interior.
Claims (10)
1. a kind of rich nitride polyporous material by bisphenol-A and melamine polycondensation, it is characterised in that：It will be to bisphenol-A and melamine
It is copolymerized in alkaline solution, generates canescence porous material PBPAM；Its specific preparation process is：Using ethylene glycol as solvent, it is added
Melamine and bisphenol-A carry out heating polycondensation, are eventually adding dimethylbenzene dehydration.
2. the rich nitride polyporous material according to claim 1 by bisphenol-A and melamine polycondensation, it is characterised in that：Trimerization
The molar ratio of cyanamide and bisphenol-A is 3:1.8~2.4.
3. the rich nitride polyporous material according to claim 1 by bisphenol-A and melamine polycondensation, it is characterised in that：Heating
The polycondensation time is 8~15 hours.
4. the rich nitride polyporous material according to claim 1 by bisphenol-A and melamine polycondensation, it is characterised in that：Heating
Temperature is 150~198 DEG C.
5. the rich nitride polyporous material according to claim 1 by bisphenol-A and melamine polycondensation, it is characterised in that：Dehydration
Time is 3-5 hours.
6. the rich nitride polyporous material according to claim 1 by bisphenol-A and melamine polycondensation, it is characterised in that：Dehydration
Temperature is 136-140 DEG C of xylene boiling point.
7. using the huge sum of money described in claim 1 by bisphenol-A and the rich nitride polyporous material absorption effluent of melamine polycondensation
Belong to the method for ion, it is characterised in that：Porous material is packed into adsorption column, heavy metal ion sewage will be contained, adsorption column is added,
Adsorption column adsorbs heavy metal ion；Then 1% diluted hydrochloric acid aqueous solution is washed into adsorption column, heavy metal ion desorption.
8. the huge sum of money according to claim 7 by bisphenol-A and the rich nitride polyporous material absorption effluent of melamine polycondensation
Belong to the method for ion, it is characterised in that：Sorbing material is 15~20 with heavy metal mass ratio in sewage：1.
9. the huge sum of money according to claim 7 by bisphenol-A and the rich nitride polyporous material absorption effluent of melamine polycondensation
Belong to the method for ion, it is characterised in that：Judge desorption terminal using atomic absorption spectrum.
10. heavy metal ion of the rich nitride polyporous material PBPAM in absorption effluent prepared by claim any one of 1-6 is answered
With.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110152630A (en) * | 2019-06-04 | 2019-08-23 | 南京信息工程大学 | A kind of new and effective adsorbent and its application |
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| CN102827368A (en) * | 2011-06-16 | 2012-12-19 | 中国科学院大连化学物理研究所 | Biomass-based organic polymer porous material and synthesizing method thereof |
| CN104910379A (en) * | 2014-03-12 | 2015-09-16 | 周卫星 | Preparation method of amino group-containing porous material, and application of amino group-containing porous material in recover of waste electric appliance precious metals |
| CN106563418A (en) * | 2015-10-09 | 2017-04-19 | 中国科学院大连化学物理研究所 | Preparation of nitrogen-enriched organic porous material, and organic porous material and application thereof |
| CN107308918A (en) * | 2017-07-14 | 2017-11-03 | 南京信息工程大学 | A kind of preparation method of rich nitride polyporous material and its in retrieving circuit board noble metal application |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102827368A (en) * | 2011-06-16 | 2012-12-19 | 中国科学院大连化学物理研究所 | Biomass-based organic polymer porous material and synthesizing method thereof |
| CN104910379A (en) * | 2014-03-12 | 2015-09-16 | 周卫星 | Preparation method of amino group-containing porous material, and application of amino group-containing porous material in recover of waste electric appliance precious metals |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110152630A (en) * | 2019-06-04 | 2019-08-23 | 南京信息工程大学 | A kind of new and effective adsorbent and its application |
| CN110152630B (en) * | 2019-06-04 | 2022-03-22 | 南京信息工程大学 | Efficient adsorbent and application thereof |
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Application publication date: 20180807 |