CN108607528A - A kind of diatomite/sulfide polymer mercury ion adsorbent and preparation method thereof - Google Patents
A kind of diatomite/sulfide polymer mercury ion adsorbent and preparation method thereof Download PDFInfo
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- CN108607528A CN108607528A CN201810429596.5A CN201810429596A CN108607528A CN 108607528 A CN108607528 A CN 108607528A CN 201810429596 A CN201810429596 A CN 201810429596A CN 108607528 A CN108607528 A CN 108607528A
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/14—Diatomaceous earth
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- 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
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- C02F2101/00—Nature of the contaminant
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Abstract
The present invention relates to sorbing material synthesis technical fields, more particularly to a kind of diatomite/sulfide polymer mercury ion adsorbent and preparation method thereof, using industrial waste sulphur, agricultural waste anacardol and diatomite as raw material, it is prepared into diatomite/sulfide polymer, diatomite/the sulfide polymer is the copolymer rich in sulphur, has high adsorption capacity to mercury ion.The present invention obtains spongiform porous polymer material.Porous polymer material has very high specific surface area, and has abundant S S functional groups, can be with faster sequestration mercury ion.There is abundant silicone hydroxyl on diatomite surface, has very strong chelating to act in heavy metal.In addition, the simple process of the present invention is easy, raw material inexpensively enriches, and without expensive equipment and harsh working condition, sorbing material all has higher adsorbance and removal rate, and will not cause secondary pollution of water, is suitble to the absorption of Mercury in Industrial Waste Water ion.
Description
Technical field
The present invention relates to sorbing material synthesis technical fields, and in particular to a kind of diatomite/sulfide polymer mercury ion suction
Enclosure material and preparation method thereof.
Background technology
Water pollution is one of the environmental problem faced at present, is badly in need of exploitation novel absorption material, so as to efficient, cheap side
Formula goes the harmful substances such as removing heavy metals.Due to exploitation of gold deposit, coal combustion, oil and natural gas refining, waste incineration, chlor-alkali,
The fields such as metallurgy, cause every year discharge thousands of tons of mercury, it was reported that be exposed to high concentration mercury can cause it is serious irreversible
Health problem, such as kidney injury, the nervous system disease and inborn defect.Just because of mercury has persistence, property easy to migrate, biology rich
The characteristics such as collection property and bio-toxicity, therefore a kind of important environmental toxic harmful substance is had become, to health and ecological ring
Cause huge threat in border.Currently, country is increasingly strict to the supervision of mercury emissions, in order to meet these regulations, it is badly in need of finding one
Kind of effective way solves mercury pollution problem, and the technology of the removal of mercury includes chemical precipitation from water system at present, ion exchange, absorption and
Membrane filtration.Compared with other methods, absorption be used as a kind of low cost, simple method and show one's talent, can effectively handle weight
The pollution problem of mercury metal has obtained universal application in fields such as environment, material, engineerings.
Cashew nut is under the jurisdiction of Anacardiaceae Anacardium, is a kind of industrial crops, originate in earliest Brazil, Asia it is coastal and African etc.
Ground is cultivated by the whole world, and there is plantation on the ground such as Yunnan Province of China, Guangxi, Guangdong, Fujian, Taiwan.Cashew nut shell oil is to process
The brown viscous liquid generated during cashew nut can obtain the derivatives of phenol a series of through vacuum distillation, including anacardol,
Cashew acid, cardol and 2- methyl cardols, wherein anacardol is the main component of cashew nut shell oil, be a kind of potentially useful again
Production-goods source has saturation or unsaturated long chain hydrocarbon groups-C15H25-31Natural phenolic compound.Contain phenyl ring in anacardol structure,
Structure is similar with phenol, phenolic hydroxyl group reaction can occur, and phenolic hydroxyl group has activated ortho para hydrogen atom on phenyl ring so that waist
Fruit phenol can react with many inorganic, organic compounds.In addition, the unsaturated bond on the long side chain alkyl of anacardol, has alkene
Oxidative polymerization can occur for the chemical feature of hydrocarbon, under certain condition, anacardol.Therefore, anacardol has become one really
Can be with regenerated fragrant phenol resource, and petroleum base phenol can be substituted and participate in a variety of chemical reactions, manufacture multiple functions
Property chemicals, is widely used to the every field such as industry, agricultural.
Sulphur be it is a kind of be easily obtained with cheap material, the annual byproduct yield as petroleum refining has been more than 5000
Ten thousand tons, however, sulphur only accounts for the 5-10% of annual output in commercial chemical drug and vulcanization of rubber usage amount, since sulphur is as danger
Incompressible entity waste of danger, therefore, in recent years, the worry to sulphur accumulation is not used has risen.
Sulphur can capture and stablize mercury, but it is chemically and physically limited by several, it is made to cannot be directly used to adsorb.Example
Such as, the burning point (190 DEG C) of element sulphur is low, is easy distillation, is easy to happen caking and increases the flowed friction in filter process, it is difficult to
It soaks and mixes in the batch processing of waste fluid, and be difficult to be prepared into the durability particle of required size.In addition, sulphur may
It is oxidized to sulfuric acid in the environment, this can increase the sulfate of the main producers of high toxicity methyl mercury in soils and sediments also
The abundance of opportunistic pathogen.Therefore, it is significantly to convert to the chemical substance of the high-affinity of mercury sulphur to.
Diatomite is that the Diatomeae grown in ocean or lake and microorganism remains are solid through operation of nature and ooze at the bottom
A kind of biological silicalite that knot is formed, diatomaceous main chemical is amorphous SiO2, and contain a small amount of Al2O3、
P2O3, CaO, MgO etc., diatom shell has natural, a large amount of, ordered arrangement hole, makes it have larger specific surface
Product, specific surface area is about 3.1-60m2/ g, hole quantity are about 2~2.5 hundred million/g, diatomite surface, internal pore surface point
It is furnished with a large amount of silicone hydroxyl, silicone hydroxyl dissociates H in aqueous solution+, so that its surface is carried certain negative electrical charge, due to its tool
There are the good characteristics such as voidage high, specific surface is big, proportion is small, wear-resisting, acidproof, strong adsorption, is widely used in diet, builds
In the industries such as material, chemical industry, the energy, water process.
We prepare diatomite/vulcanization anacardol using agriculture waste extract-anacardol and sulphur and diatomite
Polymer.The sulphur for being made of cyclic structure 8 sulphur atoms first starts to melt at 120-124 DEG C, and open loop occurs at 159 DEG C
Reaction continues to increase temperature, at 185 DEG C, forms two free radical chain of linear polythioalkane of maximum chain length, diradical and cashew nut
The monomer of phenol is copolymerized, and promotes balanced sequence, increases polythioalkane chain, generates sulfide polymer；Then, diatomite, system are added
Standby diatomite/vulcanization anacardol polymer porous material, to improve the capacity antacid and mechanical strength of material.At present with cashew nut
Phenol, sulphur and diatomite adsorb the research of mercury ion still for raw material to synthesize diatomite/vulcanization anacardol polymer porous material
It has not been reported.
Invention content
In order to solve the above technical problems, the present invention provides a kind of diatomite/sulfide polymer mercury ion adsorbent and
Preparation method effectively removes the mercury ion in water body using the function adsorbent.The present invention is directly with cheap diatomite
It is raw material with anacardol, using the sulphur of melting as solvent, NaCl is perforating agent, and raw material sources needed for the technique are abundant, prepares work
Skill is simple, cost-effective, which has the abilities such as very strong antiacid alkali resistant, and easy to use, is suitble to processing industrial wastewater
Mercury ion absorption.
Specific technical solution is as follows：
A kind of diatomite/sulfide polymer mercury ion adsorbent, with industrial waste sulphur, agricultural waste anacardol and silicon
Diatomaceous earth is raw material, is prepared into diatomite/sulfide polymer, the diatomite/sulfide polymer is the copolymer rich in sulphur, to mercury
Ion has high adsorption capacity.
A kind of preparation method of diatomite/sulfide polymer mercury ion adsorbent, specific preparation process are as follows：
(1) first by diatomite grind into powder, after the quasi- sub-sieve sieving of 200 targets, by 40% sulfuric acid by solid
Liquor ratio 1:4,80 DEG C are heated, then mechanical agitation 8h is washed with distilled water neutrality, filter, be put into drying box in 50-100
Dry at DEG C to be finally putting into inside Muffle furnace at 450 DEG C for 24 hours, heating 4h is sealed spare later；
(2) sulphur for taking 0-9g is added to round-bottomed flask, and oil bath heating is to 185 DEG C, after stirring evenly, to round-bottomed flask
The anacardol of 0-5g is added dropwise, stirs 30min, is subsequently added into the diatomite of 0-6g, is stirred under heating 10min, finally, 20g is added
NaCl is added at 10-15min, stirring in NaCl, generates thick pasty mixture, and cooling 1h takes product from flask
Go out, grinds；
(3) it takes ground above-mentioned product to be transferred to beaker, 1000ml deionized waters is then added, 1h is stirred at room temperature,
NaCl is leached from polymer, repeatedly filtering and washing, it is ensured that NaCl is removed completely, finally, is being dried in vacuo, is being finally obtained sponge
The porous polymer material of shape, is sealed product.
Compared with prior art, the method have the benefit that：
The technical scheme is that using cheap sulphur as raw material, anacardol is added, elemental sulfur is opened at appropriate temperatures
Ring generates two free radical chain of linear polythioalkane, and then the monomer of diradical and anacardol is copolymerized, and then adds difference and contains
The diatomite of amount is finally added grinding NaCl, stirs certain time for several times in batches, cooling, washes away NaCl by deionization, most
Spongiform porous polymer material is obtained eventually.Porous polymer material has very high specific surface area, and has abundant
S-S functional groups, can be with faster sequestration mercury ion.There is abundant silicone hydroxyl on diatomite surface, has very strong chelating to act in heavy metal.
In addition, the simple process of the present invention is easy, raw material inexpensively enriches, without expensive equipment and harsh working condition, adsorption material
Material all has higher adsorbance and removal rate, and will not cause secondary pollution of water, is suitble to Mercury in Industrial Waste Water ion
Absorption.
Description of the drawings
Fig. 1 is the process flow chart of diatomite-vulcanization cashew nut phenol polymer；
Fig. 2 is the SEM spectrograms of diatomite-vulcanization cashew nut phenol polymer prepared by the embodiment of the present invention 2；
Fig. 3 is the FT-IR spectrograms of diatomite-vulcanization cashew nut phenol polymer prepared by the embodiment of the present invention 3.
Specific implementation mode
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings, but protection scope of the present invention is not by attached
Figure and specific embodiment are limited.
The instrument that the present invention uses and characterizing method are as follows：FT-IR is infrared using the Spectrum One of PE companies of the U.S.
Spectrometer is tested.Solid sample uses KBr tablettings, fluid sample film on KBr chips, the wave number of absorption spectrum scanning
4000~500cm of range-1, scan 3 times.Scanning electron microscope (Scanning Electron Microscope, SEM) is using Japan's electricity
The JEOL 6500F of subsidiary.This experiment is ultraviolet using the TU-1901 dual-beams of Beijing Puxi General Instrument Co., Ltd
Visible spectrophotometer.Test method measures mercury ion content (GB7469-87) with reference to dithizone spectrophotometry
In acid mercury ion solution, Hg2+It is reacted with dithizone, generates orange chelate, maximum absorption wavelength
485nm, molar absorption coefficient 7.1 × 104L/(mol·cm).Therefore spectrophotometry can be used and measure Hg2+The absorbance of solution
Variation, and then Hg is determined according to standard curve2+Solution concentration.
The chemical reagent used in the embodiment of the present invention is provided by Sinopharm Chemical Reagent Co., Ltd.；
The diatomite used in the embodiment of the present invention comes from Changbai area；
With reference to specific embodiment, elaborate to the present invention.These embodiments be merely to illustrate the present invention without
Application range for limiting the present invention.Such equivalent forms are made various changes or modifications etc. equally in the application institute to the present invention
The range that attached claims are limited.
Embodiment 1：
Fig. 1 is the process flow chart of diatomite-vulcanization cashew nut phenol polymer, as shown in the figure：
(1) first by diatomite grind into powder, after the quasi- sub-sieve sieving of 200 targets, by 40% sulfuric acid by solid
Liquor ratio 1:4, mechanical agitation heats 80 DEG C, handles 8h, is then washed with distilled water neutrality, filters, is put into drying box in 50
It is dry at DEG C to be finally putting into inside Muffle furnace at 450 DEG C for 24 hours, it is sealed after heating 4h spare；
(2) 9g sulphur is taken, 250ml round-bottomed flasks are added to, oil bath heating forms orange solution to 185 DEG C, then, to
1g anacardols are added dropwise in round-bottomed flask, stir 30min, are subsequently added into 0g diatomite, are stirred under heating 10min, finally, 20g are added
The NaCl ground in advance adds 4 NaCl, each 5g in 10min, generates thick pasty mixture, cooling 1h, product from
It takes out, grinds in flask.
(3) it takes ground product to be transferred to 1000ml beakers, a certain amount of deionized water is then added, is stirred at room temperature
1h leaches NaCl from polymer, and filtering and washing, then, washing is multiple in an identical manner, to ensure that NaCl goes out completely,
Finally, it is being dried in vacuo, is finally obtaining spongiform porous polymer material, be sealed product.The adsorbance of product at this time
For 50.26mg/g, by the sem analysis of Fig. 2 materials, diatomite-vulcanization cashew nut phenol polymer shows the smooth surface in part, and
And there is abundant pore passage structure.
Embodiment 2：
(1) identical as step (1) synthesis in embodiment 1, the drying temperature being put into drying box is 60 DEG C；
(2) 7g sulphur is taken, 250ml round-bottomed flasks are added to, oil bath heating forms orange solution to 185 DEG C, then, to
3g anacardols are added dropwise in round-bottomed flask, stir 30min, are subsequently added into 0g diatomite, are stirred under heating 10min, finally, 20g are added
The NaCl ground in advance adds 4 NaCl, each 5g in 10min, generates thick pasty mixture, cooling 1h, product from
It takes out, grinds in flask；
(3) identical as step (3) synthesis in embodiment 1；The adsorbance of product is 60.47mg/g at this time.Fig. 2 is the present invention
The SEM spectrograms of diatomite-vulcanization cashew nut phenol polymer prepared by embodiment 2, pass through the sem analysis of Fig. 2 materials, diatomite-sulphur
Change the smooth surface in cashew nut phenol polymer display part, and there is abundant pore passage structure.
Embodiment 3：
(1) identical as step (1) synthesis in embodiment 1, the drying temperature being put into drying box is 70 DEG C；
(2) 5g sulphur is taken, 250ml round-bottomed flasks are added to, oil bath heating forms orange solution to 185 DEG C, then, to
5g anacardols are added dropwise in round-bottomed flask, stir 30min, are subsequently added into 0g diatomite, are stirred under heating 10min, finally, 20g are added
The NaCl ground in advance adds 4 NaCl, each 5g in 10min, generates thick pasty mixture, cooling 1h, product from
It takes out, grinds in flask；
(3) identical as step (1) synthesis in embodiment 1；The adsorbance of product is 53.12mg/g at this time.Fig. 3 is the present invention
The FT-IR spectrograms of diatomite-vulcanization cashew nut phenol polymer prepared by embodiment 3, by the FT-IR spectrum analysis of Fig. 3 materials,
1090cm-1And 806cm-1The characteristic peak of appearance is belonging respectively to Si-O stretching vibrations and Si-O-Si symmetrical stretching vibrations, meets silicon
The SiO of diatomaceous earth2Infrared signature peak.In addition, in 1595cm-1And 1455cm-1Place is the skeletal vibration of the phenyl ring of anacardol,
658cm-1Characteristic peak belong to C-S, it was demonstrated that formd sulfur-bearing co-polymer, therefore, met experimental design requirement.
Embodiment 4：
(1) identical as step (1) synthesis in embodiment 1, the drying temperature being put into drying box is 75 DEG C；
(2) 9g sulphur is taken, 250ml round-bottomed flasks, oil bath heating to 185 are added to℃, form orange solution, then, Xiang Yuan
1g anacardols are added dropwise in bottom flask, stir 30min, are subsequently added into 1g diatomite, are stirred under heating 10min, finally, it is pre- that 20g are added
The NaCl first ground adds 4 NaCl, each 5g in 12min, generates thick pasty mixture, cooling 1h, and product is from burning
It takes out, grinds in bottle；
(3) identical as step (1) synthesis in embodiment 1；The adsorbance of product is 66.85mg/g at this time.
Embodiment 5：
(1) identical as step (1) synthesis in embodiment 1, the drying temperature being put into drying box is 80 DEG C；
(2) 7g sulphur is taken, 250ml round-bottomed flasks are added to, oil bath heating forms orange solution to 185 DEG C, then, to
3g anacardols are added dropwise in round-bottomed flask, stir 30min, are subsequently added into 1g diatomite, are stirred under heating 10min, finally, 20g are added
The NaCl ground in advance adds 4 NaCl, each 5g in 12min, generates thick pasty mixture, cooling 1h, product from
It takes out, grinds in flask；
(3) identical as step (1) synthesis in embodiment 1；The adsorbance of product is 70.29mg/g at this time.
Embodiment 6：
(1) identical as step (1) synthesis in embodiment 1, the drying temperature being put into drying box is 85 DEG C；
(2) 5g sulphur is taken, 250ml round-bottomed flasks, oil bath heating to 185 are added to℃, form orange solution, then, Xiang Yuan
5g anacardols are added dropwise in bottom flask, stir 30min, are subsequently added into 1g diatomite, are stirred under heating 10min, finally, it is pre- that 20g are added
The NaCl first ground adds 4 NaCl, each 5g in 12min, generates thick pasty mixture, cooling 1h, and product is from burning
It takes out, grinds in bottle；
(3) identical as step (1) synthesis in embodiment 1；The adsorbance of product is 63.76mg/g at this time.
Embodiment 7：
(1) identical as step (1) synthesis in embodiment 1, the drying temperature being put into drying box is 90 DEG C；
(2) 9g sulphur is taken, 250ml round-bottomed flasks are added to, oil bath heating forms orange solution to 185 DEG C, then, to
1g anacardols are added dropwise in round-bottomed flask, stir 30min, are subsequently added into 2g diatomite, are stirred under heating 10min, finally, 20g are added
The NaCl ground in advance adds 4 NaCl, each 5g in 15min, generates thick pasty mixture, cooling 1h, product from
It takes out, grinds in flask；
(3) identical as step (1) synthesis in embodiment 1；The adsorbance of product is 71.84mg/g at this time.
Embodiment 8：
(1) identical as step (1) synthesis in embodiment 1, the drying temperature being put into drying box is 95 DEG C；
(2) 7g sulphur is taken, 250ml round-bottomed flasks, oil bath heating to 185 are added to℃, form orange solution, then, Xiang Yuan
3g anacardols are added dropwise in bottom flask, stir 30min, are subsequently added into 2g diatomite, are stirred under heating 10min, finally, it is pre- that 20g are added
The NaCl first ground adds 4 NaCl, each 5g in 15min, generates thick pasty mixture, cooling 1h, and product is from burning
It takes out, grinds in bottle；
(3) identical as step (1) synthesis in embodiment 1；The adsorbance of product is 78.21mg/g at this time.
Embodiment 9：
(1) identical as step (1) synthesis in embodiment 1, the drying temperature being put into drying box is 100 DEG C；
(2) 5g sulphur is taken, 250ml round-bottomed flasks are added to, oil bath heating forms orange solution to 185 DEG C, then, to
5g anacardols are added dropwise in round-bottomed flask, stir 30min, are subsequently added into 2g diatomite, are stirred under heating 10min, finally, 20g are added
The NaCl ground in advance adds 4 NaCl, each 5g in 15min, generates thick pasty mixture, cooling 1h, product from
It takes out, grinds in flask；
(3) identical as step (1) synthesis in embodiment 1；The adsorbance of product is 74.33mg/g at this time.
It can be seen that the sorbing material has higher adsorbance, the absorption of Mercury in Industrial Waste Water ion can be met.
Claims (2)
1. a kind of diatomite/sulfide polymer mercury ion adsorbent, it is characterised in that：With industrial waste sulphur, agricultural waste
Anacardol and diatomite are raw material, are prepared into diatomite/sulfide polymer, and the diatomite/sulfide polymer is rich in sulphur
Copolymer has high adsorption capacity to mercury ion.
2. a kind of preparation method of diatomite/sulfide polymer mercury ion adsorbent, which is characterized in that specific preparation process is such as
Under：
(1) diatomite grind into powder is pressed into solid-to-liquid ratio after the quasi- sub-sieve sieving of 200 targets by 40% sulfuric acid first
1:4,80 DEG C are heated, then mechanical agitation 8h is washed with distilled water neutrality, filter, be put into drying box at 50-100 DEG C
Dry to be finally putting into inside Muffle furnace at 450 DEG C for 24 hours, heating 4h is sealed spare later；
(2) sulphur for taking 0-9g is added to round-bottomed flask, and oil bath heating is to 185 DEG C, after stirring evenly, is added dropwise to round-bottomed flask
The anacardol of 0-5g stirs 30min, is subsequently added into the diatomite of 0-6g, is stirred under heating 10min, finally, 20g is added
NaCl is added at 10-15min, stirring in NaCl, generates thick pasty mixture, and cooling 1h takes product from flask
Go out, grinds；
(3) it takes ground above-mentioned product to be transferred to beaker, 1000ml deionized waters is then added, 1h is stirred at room temperature, from poly-
It closes in object and leaches NaCl, repeatedly filtering and washing, it is ensured that NaCl is removed completely, finally, is being dried in vacuo, is being finally obtained spongiform
Porous polymer material is sealed product.
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| CN110586023A (en) * | 2019-09-20 | 2019-12-20 | 中国科学院地球化学研究所 | Sulfur-modified chalcopyrite adsorbing material, preparation method and application thereof |
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