CN109046294A - A kind of preparation method for the nano thin-film removing heavy metal in waste water mercury ion - Google Patents

A kind of preparation method for the nano thin-film removing heavy metal in waste water mercury ion Download PDF

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Publication number
CN109046294A
CN109046294A CN201811024717.4A CN201811024717A CN109046294A CN 109046294 A CN109046294 A CN 109046294A CN 201811024717 A CN201811024717 A CN 201811024717A CN 109046294 A CN109046294 A CN 109046294A
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CN
China
Prior art keywords
waste water
mercury ion
film
heavy metal
preparation
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
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CN201811024717.4A
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Chinese (zh)
Inventor
舒黎幼
邵明
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Sharp Bio Tech Ltd Suzhou One Hundred
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Sharp Bio Tech Ltd Suzhou One Hundred
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Priority to CN201811024717.4A priority Critical patent/CN109046294A/en
Publication of CN109046294A publication Critical patent/CN109046294A/en
Pending legal-status Critical Current

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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
    • B01J20/28014—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 form
    • B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
    • 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
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • 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
    • B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
    • 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
    • B01J20/28004—Sorbent size or size distribution, e.g. particle size
    • B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
    • 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
    • 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
    • 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
    • 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
    • B01J2220/46—Materials comprising a mixture of inorganic and organic materials
    • 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

Abstract

The present invention relates to a kind of preparation methods of nano thin-film for removing heavy metal in waste water mercury ion, and step includes: the preparation of (1) nano thin-film；(2) mercury ion is adsorbed from waste water using nano thin-film, the elution of mercury ion after absorption；(3) test absorption front and back, the adsorbance of mercury ion.This method is simple, efficient, suitable for quickly removing the metal mercury ions waste water.

Description

A kind of preparation method for the nano thin-film removing heavy metal in waste water mercury ion
Technical field
The invention belongs to the application fields of Environmental Chemistry, the in particular to minimizing technology of heavy metal ions in wastewater.
Background technique
With the rapid development of industry, heavy metal ion pollution has seriously affected human society survival and development and has formed For the hot issue of World Focusing.Mercury ion in environment is easy to enter in human body by food chain, can make to human health At serious threat, it can cause to have a headache, have difficulty in breathing, cause intravascular hemolysis, injuring nerve system, based on these harm, people Have studied a variety of methods to administer mercury ion waste liquid.Oneself is had investigated various ways to remove mercury ion to people, Such as the filtering of the precipitation method, film, ion exchange, electrolysis method and absorption method, wherein absorption method is the most common method of people, this Method operation is terse, and energy consumption is few, and expense is low, it is most important that removal rate is high.Nano material in adsorbent material has many suctions Attached advantage, therefore by favor.Nano thin-film is a kind of material of nanometer-scale, and because of its simple process, absorption property is good, is convenient for The advantages of separation, and be widely used.
Graphene oxide contains a large amount of adsorption functional group as a kind of derivative of graphene, is promptly widely applied In many fields, paid much attention in environmental area by scholar, it is a kind of monoatomic layer structure, has high surface area, surface contains Have the groups such as a large amount of hydroxyl, carboxyl, epoxy group, and be both exposed to surface, low manufacture cost, good water solubility, can with again Chelation occurs for metal.Graphene oxide is difficult the recycling that is separated after having handled metal ion, therefore, looks for one Kind substance is a kind of very good solution method as carrier.Electrostatic spinning technique may be implemented it is organic with it is inorganic compound, make fiber Film has both organic and inorganic advantage, and the electrostatic spinning fiber film large specific surface area produced, and porosity is high, provides for absorption Good physical structure.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of method that removal heavy metal in waste water leads to ion, this method It is time-consuming less using the method for Static Adsorption using polyacrylonitrile/graphene oxide composite nano film as adsorbent, it can Quickly, metal mercury ions are adsorbed in the slave waste water of high dose；The prices of raw materials used in the present invention are cheap, and obtained answers Nano thin-film surface area with higher is closed, adsorption capacity is strong, the potentiality with subsequent related application.
A kind of preparation method of the nano thin-film of removal heavy metal in waste water mercury ion of the invention, comprising:
(1) a certain amount of polyacrylonitrile (PAN) powder is weighed, is dissolved into the DMF solution containing graphene oxide (GO), room Temperature lower stirring 30 ~ 50 hours, obtain uniform, the transparent PAN spinning solution containing GO.At room temperature, the blend spinning that will be prepared Liquid is placed in disposable syringe, the syringe with syringe needle is fixed on the feed system of electrostatic spinning equipment, is spun Silk, is prepared the composite nano film of GO/PAN.
(2) composite nano film prepared in a certain amount of step (1) is added in certain density mercury-containing waste water, It under conditions of room temperature and certain pH value, reacts certain time, the concentration of test absorption front and back mercury ion calculates adsorbance.
PAN mass concentration is 5-10 wt.% in the step (1).
GO mass is 2-8 wt.% in the step (1).
Spinning voltage is 10-20 KV in the step (1).
Flow velocity 0.5-2.0 mL/h is sprayed in the step (1).
Mercury ion solution concentration is 20 ~ 500 mg/L in the step (2).
The pH value of solution is 3 ~ 10 in the step (2).
The reaction time of solution is 2 ~ 5 h in the step (2).
Beneficial effect
(1) composite nano film prepared by the present invention, it is easy to operate, it is easy to industrial amplification；
(2) composite nano film prepared by the present invention has biggish specific surface area and preferable absorption property, can be quick, high Metal mercury ions are adsorbed in the slave waste water of dosage；
Detailed description of the invention
Fig. 1 is adsorbance of the nano thin-film to mercury ion.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited Range.
Embodiment 1
The preparation of polyacrylonitrile/graphene oxide composite nanometer film, includes the following steps:
A certain amount of PAN powder is weighed, is dissolved into the DMF solution containing graphene oxide, stirs 48 hours, obtains at room temperature PAN mass fraction is 8%, the uniform spinning solution of graphene oxide mass fraction 5%.At room temperature, the blend spinning that will be prepared Liquid is placed in 10 disposable syringe, the syringe with syringe needle is fixed on the feed system of electrostatic spinning equipment, is spun Filament voltage selects 15 KV, sprays 1.0 ml/h of flow velocity, receives distance 10cm, and one layer of aluminium foil of paving, which is used as, on the reception device receives Plate, finally by composite nano film obtained in empty drying box dry 24 hours to get.
Embodiment 2
Composite nano film includes the following steps: the adsorption experiment of mercury ion
100 mL of mercury ion solution of the mg/L of 30 mg/L ~ 400 is measured respectively in 150 mL beakers, accurately weighs more parts of changes 0.05 g composite nano film, is put in beaker, adjust pH be 5, shake 3 h at room temperature, then detection absorption after mercury from Adsorbance qe is calculated as follows in sub- concentration.
Qe=(C0-C1) V/m
In formula, C0, Ct are respectively indicated ion concentration of mercury in initial soln (mg/L), and C1 is that oscillation terminates metal in rear solution Ion concentration (mg/L), V are the volume (L) of aqueous solution, and m is the quality (g) of composite nano film.
Fig. 1 reflects influence of the concentration to absorption, the adsorbance of nano thin-film with ion concentration of mercury in solution increase And increase, until absorption reaches balance.When ion concentration of mercury is lower, the adsorbance of adsorbent is less, this may be because Under low concentration, the adsorption site on nano thin-film is not fully utilized；And with the increase of ion concentration of mercury, it is non-full on adsorbent Continue with the adsorption site of state and mercury ion combines, to make adsorbance increase, until absorption reaches balance.From figure we It can also be seen that adsorbent is 63.7mg/g to the maximum saturation adsorbance of mercury ion, illustrate that adsorbent of the invention is this Kind of adsorption capacity is big, efficient adsorbent for heavy metal.

Claims (6)

1. a kind of preparation method for the nano thin-film for removing heavy metal in waste water mercury ion, including the following steps:
(1) a certain amount of polyacrylonitrile (PAN) powder is weighed, is dissolved into the DMF solution containing graphene oxide (GO), room Temperature lower stirring 30 ~ 50 hours, obtain uniform, the transparent PAN spinning solution containing GO；At room temperature, the blend spinning that will be prepared Liquid is placed in disposable syringe, the syringe with syringe needle is fixed on the feed system of electrostatic spinning equipment, is spun Silk, is prepared the composite nano film of GO/PAN；
(2) composite nano film prepared in a certain amount of step (1) is added in certain density mercury-containing waste water, in room temperature And under conditions of certain pH value, react certain time, the concentration of test absorption front and back mercury ion calculates adsorbance.
2. a kind of preparation method of nano thin-film for removing heavy metal in waste water mercury ion according to claim 1, special Sign is that the PAN mass concentration as described in step (1) is 5-10 wt.%.
3. a kind of preparation method of nano thin-film for removing heavy metal in waste water mercury ion according to claim 1, special Sign is that GO mass is 2-8 wt.% in the step (1).
4. a kind of preparation method of nano thin-film for removing heavy metal in waste water mercury ion according to claim 1, special Sign is that the attacking system of electrostatic spinning system in the step (1), spinning voltage is 10-20 KV, sprays flow velocity 0.5-2.0 mL/h、。
5. a kind of preparation method of quick adsorption heavy metal in waste water mercury ion according to claim 1, feature exist In mercury ion solution concentration is 20 ~ 500 mg/L in the step (2).
6. a kind of preparation method of quick adsorption heavy metal in waste water mercury ion according to claim 1, feature exist In the pH value of solution is 3 ~ 10 in the step (2), and the reaction time is 2 ~ 5 h.
CN201811024717.4A 2018-09-04 2018-09-04 A kind of preparation method for the nano thin-film removing heavy metal in waste water mercury ion Pending CN109046294A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111018037A (en) * 2019-12-19 2020-04-17 上海交通大学 Method for removing heavy metal mercury ions in water based on polyacrylonitrile nano-film compound

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103663601A (en) * 2013-08-05 2014-03-26 南昌大学 Method for absorptively separating low-concentration heavy-metal ions by utilizing graphene oxide colloid
CN105457603A (en) * 2015-11-02 2016-04-06 上海交通大学 Nano-fiber for adsorbing heavy metal ions and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103663601A (en) * 2013-08-05 2014-03-26 南昌大学 Method for absorptively separating low-concentration heavy-metal ions by utilizing graphene oxide colloid
CN105457603A (en) * 2015-11-02 2016-04-06 上海交通大学 Nano-fiber for adsorbing heavy metal ions and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
刘甜甜: "聚丙烯腈基纳米纤维的制备及其对铜离子吸附性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111018037A (en) * 2019-12-19 2020-04-17 上海交通大学 Method for removing heavy metal mercury ions in water based on polyacrylonitrile nano-film compound

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Application publication date: 20181221