CN106745455A - A kind of method of mercury ion in functionalization superfine fibre quick adsorption water based on thiocarbamide - Google Patents
A kind of method of mercury ion in functionalization superfine fibre quick adsorption water based on thiocarbamide Download PDFInfo
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- CN106745455A CN106745455A CN201611135881.3A CN201611135881A CN106745455A CN 106745455 A CN106745455 A CN 106745455A CN 201611135881 A CN201611135881 A CN 201611135881A CN 106745455 A CN106745455 A CN 106745455A
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- thiocarbamide
- mercury ion
- superfine fibre
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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
-
- 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
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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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
- B01J20/28023—Fibres or filaments
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/402—Amides imides, sulfamic acids
- D06M13/432—Urea, thiourea or derivatives thereof, e.g. biurets; Urea-inclusion compounds; Dicyanamides; Carbodiimides; Guanidines, e.g. dicyandiamides
-
- 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
- B01J2220/44—Materials comprising a mixture of organic materials
- B01J2220/445—Materials comprising a mixture of organic materials comprising a mixture of polymers
-
- 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
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
-
- 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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Textile Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a kind of method of mercury ion in functionalization superfine fibre quick adsorption water based on thiocarbamide, it is related to a kind of preparation and application of thiocarbamide functionalization superfine fibre, belongs to functional material and heavy metal quick adsorption processing technology field.Specifically the thiocarbamide for having strong ligand complex ability to mercury ion is modified to matrix fiber material, using the method for mercury ion in the Static Adsorption removal aqueous solution.The present invention can thoroughly remove mercury ion in the aqueous solution, and with sorbing material wide material sources, with low cost, simple to operate, removal quickness and high efficiency, selectivity are high, the advantages of adsorption capacity is big.
Description
Technical field
The present invention relates to functional material and heavy metal quick adsorption processing technology field, specifically, it is related to one kind to be based on
The method of mercury ion in thiocarbamide functionalization superfine fibre quick adsorption water.
Background technology
With the fast development of global industry, especially intermetallic composite coating, plating, battery etc. be related to heavy metal containing high concentration from
The rise of sub- waste water industry, heavy metal pollution is increasingly serious in causing water body environment, and most common of which is exactly heavy metal Hg
Pollution.Mercury ion enters water by the separate sources such as the burning and waste of fossil fuel and medicine, fluorescent product, thermometer
Body environment, its biodegradability is poor, can be enriched in human organ by food chain, causes neurotrosis, ataxia, depending on
Power declines, and hearing weakens, the symptom such as anxious state of mind, and heart failure can be caused when serious, or even dead, and the death rate is up to 40%.
Therefore, it is the living environment of the beautification mankind, reduces health hazard, minimizes Hg in waste water2+Concentration, reaches country's discharge mark
Standard, is current problem demanding prompt solution.
Absorption method, due to low cost, good adsorption performance, is most simple, effectively removal heavy metal in water ion method
One of.Chelate fibre is the ion-exchange fibre of the functional group for having special adsorption capacity containing heavy metal ion.Compare
Compared with other adsorbents, due to the introducing of chelating functional group, it is set to have that adsorption capacity is high, the rate of adsorption is fast, that selectivity is good is excellent
Benign energy, meanwhile, chelate fibre also has the advantages such as specific surface area is big, absorption power is high, sorbing material is with low cost, by phase
The great attention of pass field scholar.
There are lone pair electrons in thiocarbamide molecule on S and N atoms, co-ordination complex can be formed with mercury ion.The present invention is poly-
On the basis of acrylic acid-grafted polypropylene superfine fibre, by amide condensed dose with the condensation reaction of thiocarbamide, will be to Hg2+Ion has
There is the thiourea modified on superfine fibre surface of height complexing power, realize and quick, the efficient absorption of Mercury in Water Body ion are gone
Remove.
The content of the invention
It is an object of the invention to provide it is a kind of based on thiocarbamide functionalization superfine fibre it is environmentally friendly, efficient and economical and practical,
The easy mercury ion Adsorption method of synthesis technique, the material has excellent mercury ion absorption property, can be inhaled using static
The mercury ion that attached method is gone in water removal, does not result in secondary pollution after use.
The technical solution adopted in the present invention is as follows：
It is then anti-with thiocarbamide again first using the amide condensed dose of polypropylene superfine fiber of activated polyacrylic acid graft modification
Thiocarbamide functionalization superfine fibre should be prepared, and there is provided the fiber under the conditions of certain pH value, by adsorb remove in water mercury from
The method of son.
The method of mercury ion, comprises the following steps in a kind of functionalization superfine fibre quick adsorption water based on thiocarbamide：
A. the preparation of thiocarbamide functionalization superfine fibre
1) activation stage：Polyacrylic acid grafted modified polypropylene superfine fiber is inserted in beaker with amide condensed dose,
The two is added according to superfine fibre carboxyl-content with amide condensed dose of mol ratio 1: 1~2, takes the cushioning liquid of certain pH value, plus
In entering beaker, 0.5~3h of stirring reaction at 25 DEG C of room temperature；
2) the amidation process stage：The superfine fibre of above-mentioned activation is placed in the cushioning liquid of certain pH, according to acid amides
Condensing agent：Thiocarbamide mol ratio is 1: 1~2 addition thiocarbamides, at room temperature 1~6h of stirring reaction, and question response terminates, with ultra-pure water and nothing
Water-ethanol washing is multiple, to remove the monomer and homopolymers being attached on fiber, is vacuum dried at 40 DEG C, standby；
B. in water mercury ion quick adsorption application
A certain amount of thiocarbamide functionalization superfine fibre is taken, is placed in the mercury ion aqueous solution, adjust solution ph, stirring is inhaled
It is attached.
It is an advantage of the invention that：
1) active group of functionalization superfine fibre is present in fiber surface mostly, reduces the diffusion process of ion, fine
The physical aspect for tieing up shape makes it have larger contact area with adsorbate, and smaller to the resistance of fluid, substantially increase from
The speed that son is exchanged, adsorbance is big, efficiency high, and easy to use, it is easy to reclaim；
2) using thiocarbamide and mercury ion complexing stability constant advantage high, thiocarbamide functional modification is existed by chemical modification
Superfine fibre surface, substantially increases the affinity of fiber surface and mercury ion, improves adsorption capacity and removal efficiency.
3) preparation process is simple of the invention, it is with low cost, be easy to extensive preparation, functionalization material can by mercury in water from
Sub thoroughly removal, the absorption for being applied to mercury-containing waste water is removed and has that simple to operate, low cost, clearance be high, selectivity is good.
Specific embodiment
Following examples will be further described to the present invention, but not thereby limiting the invention.
Embodiment 1
A. the preparation of thiocarbamide functionalization superfine fibre
1) activation stage：By the polyacrylic acid grafted modified polypropylene superfine fibers (carboxyl-content 0.0058mol) of 1.0g,
0.0058mol1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides and 0.0058mol N-hydroxy-succinamides
In the beaker being added to, the cushioning liquid of 100mLpH 6.0 is measured, at room temperature stirring reaction 0.5h；
2) the amidation process stage：Above-mentioned activated fiber is placed in the cushioning liquid of 100mL pH 7.2, and is added
The thiocarbamide of 0.0058mol, is stirred at room temperature reaction 2h after being well mixed, question response terminates, washed with ultra-pure water and absolute ethyl alcohol
Wash repeatedly, to remove the monomer and homopolymers being attached on fiber, be vacuum dried at 40 DEG C, it is standby.
B. in water mercury ion quick adsorption application
The thiocarbamide functionalization superfine fibre of 50mg is weighed, is placed in 50mL10mg/L mercury ion water, pH value is adjusted to 5, constant temperature
25 DEG C, water-bath vibration 2h takes out, and functionalization chelate fibre is 10mg/g to the equilibrium adsorption capacities of mercury ion, and clearance is 95%
More than.
Embodiment 2
A. the preparation of thiocarbamide functionalization superfine fibre
1) activation stage：By the polyacrylic acid grafted modified polypropylene superfine fibers (carboxyl-content 0.015mol) of 5.0g,
In the beaker that 0.015mol dicyclohexylcarbodiimides are added to, the cushioning liquid of 200mLpH 5 is measured, at room temperature stirring reaction
1h；
2) the amidation process stage：Above-mentioned activated fiber is placed in the cushioning liquid of 100mLpH 6.8, and is added
The thiocarbamide of 0.045mol, is stirred at room temperature reaction 4h after being well mixed, question response terminates, with ultra-pure water and absolute ethanol washing
Repeatedly, to remove the monomer and homopolymers being attached on fiber, it is vacuum dried at 40 DEG C, it is standby.
B. in water mercury ion quick adsorption application
The thiocarbamide functionalization superfine fibre of 100mg is weighed, is placed in 100mL20mg/L mercury ion water, pH value is adjusted to 6, perseverance
25 DEG C of temperature, water-bath vibration 10min takes out, and functionalization chelate fibre is 10.8mg/g, removal to the equilibrium adsorption capacities of mercury ion
Rate is more than 96%.
Embodiment 3
A. the preparation of thiocarbamide functionalization superfine fibre
1) activation stage：By the polyacrylic acid grafted modified polypropylene superfine fibers (carboxyl-content 0.02mol) of 1.0g,
In the beaker that 0.04mol N, N '-DIC are added to, the cushioning liquid of 100mLpH 8 is measured, stirred at room temperature
Mix reaction 2h；
2) the amidation process stage：Above-mentioned activated fiber is placed in the cushioning liquid of 100mL pH 5.6, and is added
The thiocarbamide of 0.08mol, is stirred at room temperature reaction 3h after being well mixed, question response terminates, with ultra-pure water and absolute ethanol washing
Repeatedly, to remove the monomer and homopolymers being attached on fiber, it is vacuum dried at 40 DEG C, it is standby.
B. in water mercury ion quick adsorption application
The thiocarbamide functionalization superfine fibre of 50mg is weighed, is placed in 100mL10mg/L mercury ion water, pH value is adjusted to 5, constant temperature
25 DEG C, water-bath vibration 10min takes out, and functionalization chelate fibre is 11.2mg/g, clearance to the equilibrium adsorption capacities of mercury ion
More than 97%.
Embodiment 4
A. the preparation of thiocarbamide functionalization superfine fibre
1) activation stage：By the polyacrylic acid grafted modified polypropylene superfine fibers (carboxyl-content 0.04mol) of 2.0g,
0.06mol1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides and 0.06mol N-hydroxy-succinamides are added
To beaker in, measure the cushioning liquid of 100mLpH 6.0, at room temperature stirring reaction 1h；
2) the amidation process stage：Above-mentioned activated fiber is placed in the cushioning liquid of 100mL pH 7.2, and is added
The thiocarbamide of 0.12mol, is stirred at room temperature reaction 2h after being well mixed, question response terminates, with ultra-pure water and absolute ethanol washing
Repeatedly, to remove the monomer and homopolymers being attached on fiber, it is vacuum dried at 40 DEG C, it is standby.
B. in water mercury ion quick adsorption application
The thiocarbamide functionalization superfine fibre of 50mg is weighed, is placed in 50mL10mg/L mercury ion water, pH value is adjusted to 6, constant temperature
25 DEG C, water-bath vibration 10min takes out, and functionalization chelate fibre is 11.6mg/g, clearance to the equilibrium adsorption capacities of mercury ion
More than 98%.
Claims (6)
1. in a kind of functionalization superfine fibre quick adsorption water based on thiocarbamide mercury ion method, including the ultra-fine fibre of thiocarbamide functionalization
The application of mercury ion quick adsorption, specific as follows in the preparation of dimension and water：
A. the preparation of thiocarbamide functionalization superfine fibre
1) activation stage：Polyacrylic acid grafted modified polypropylene superfine fiber is inserted in beaker with amide condensed dose, the two
Added with amide condensed dose of mol ratio 1: 1~2 according to superfine fibre carboxyl-content, take the cushioning liquid of certain pH value, added and burn
In cup, 0.5~3h of stirring reaction at 25 DEG C of room temperature；
2) the amidation process stage：The superfine fibre of above-mentioned activation is placed in the cushioning liquid of certain pH, according to amide condensed
Agent：Thiocarbamide mol ratio is 1: 1~2 addition thiocarbamides, at room temperature 1~6h of stirring reaction, and question response terminates, with ultra-pure water and anhydrous second
Alcohol washing is multiple, to remove the monomer and homopolymers being attached on fiber, is vacuum dried at 40 DEG C, standby；
B. in water mercury ion quick adsorption application
A certain amount of thiocarbamide functionalization superfine fibre is taken, is placed in the mercury ion aqueous solution, adjust solution ph, stirring and adsorbing.
2. according to claim 1, it is characterised in that the polyacrylic acid grafted modified polypropylene in step a used by activation stage
Superfine fibre grafting rate is 10~200% (wt%).
3. according to claim 1, it is characterised in that amide condensed dose in step a used by activation stage is 1- (3- dimethylaminos
Propyl group) -3- ethyl-carbodiimide hydrochlorides, N-hydroxy-succinamide, dicyclohexylcarbodiimide, N, N '-diisopropyl carbon
One or more in diimine.
4. according to claim 1, it is characterised in that the cushioning liquid in step a used by activation stage is by 2- (N- morpholines) second sulphur
Acid is formulated with water, and concentration is 0.05~0.3mol/L, and pH is 3.0~8.2.
5. according to claim 1, it is characterised in that the cushioning liquid in step a used by the amidation process stage is by biphosphate
Sodium, disodium hydrogen phosphate and water are formulated, and concentration is 0.05~0.5mol/L, and pH is 4.8~9.4.
6., according to claim 1, it is characterised in that the pH value of solution is allocated with NaOH and HCl in step b, pH is 2~8.
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| CN201611135881.3A CN106745455A (en) | 2016-12-08 | 2016-12-08 | A kind of method of mercury ion in functionalization superfine fibre quick adsorption water based on thiocarbamide |
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| CN201611135881.3A CN106745455A (en) | 2016-12-08 | 2016-12-08 | A kind of method of mercury ion in functionalization superfine fibre quick adsorption water based on thiocarbamide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113398889A (en) * | 2021-06-10 | 2021-09-17 | 广西大学 | Multi-adsorption-site type biomass-based hyperbranched multi-metal ion adsorption material and preparation method and application thereof |
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| CN103301817A (en) * | 2013-05-03 | 2013-09-18 | 浙江工商大学 | Chelate fiber ABTF and synthetic method thereof |
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2016
- 2016-12-08 CN CN201611135881.3A patent/CN106745455A/en active Pending
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| JP2002336818A (en) * | 2001-05-17 | 2002-11-26 | Tamura Kagaku Kenkyusho:Kk | Method for treating processing residue of mollusk food, treatment process and treatment device used therefor |
| CN102140705A (en) * | 2010-12-24 | 2011-08-03 | 吉林大学 | Method for preparing thioamide-based chelating nanofiber for adsorbing heavy metal ions |
| CN102493187A (en) * | 2011-12-12 | 2012-06-13 | 沈阳化工大学 | Method for producing polypropylene-based ion-chelating fibers capable of absorbing heavy metal ions |
| CN103301817A (en) * | 2013-05-03 | 2013-09-18 | 浙江工商大学 | Chelate fiber ABTF and synthetic method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113398889A (en) * | 2021-06-10 | 2021-09-17 | 广西大学 | Multi-adsorption-site type biomass-based hyperbranched multi-metal ion adsorption material and preparation method and application thereof |
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