CN103055819B - A kind of heavy metal absorbent and Synthesis and applications thereof - Google Patents
A kind of heavy metal absorbent and Synthesis and applications thereof Download PDFInfo
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- CN103055819B CN103055819B CN201310033193.6A CN201310033193A CN103055819B CN 103055819 B CN103055819 B CN 103055819B CN 201310033193 A CN201310033193 A CN 201310033193A CN 103055819 B CN103055819 B CN 103055819B
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- heavy metal
- aminopropyl triethoxysilane
- oligomeric
- metal absorbent
- graphite oxide
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Abstract
A kind of heavy metal absorbent and Synthesis and applications thereof; The present invention relates to a kind of composite-Graphene-oligomeric 3-aminopropyl triethoxysilane, and Graphene-oligomeric 3-aminopropyl triethoxysilane composite is used as heavy metal absorbent by the present invention.Heavy metal absorbent of the present invention has excellent performance in heavy metal containing wastewater treatment.
Description
Technical field
The present invention relates to a kind of preparations and applicatio of heavy metal absorbent.
Background technology
What industrial expansion brought is wealth is also various hidden danger.Wherein heavy metal pollution is to badly influence the life of the mankind.Therefore, the purified treatment of heavy metal waste water has become one of problem demanding prompt solution in environmental protection.Absorption method is an important means of process heavy metal pollution, and current existing heavy metal absorbent has inorganic adsorbing material as active carbon, vermiculite, bentonite etc., organic adsorption material cellulose and modified product, shitosan etc.There is heavy metal adsorption limited capacity or the shortcoming such as mechanical performance is bad in these sorbing materials.
Summary of the invention
Object of the present invention is intended to adsorbent and the Synthesis and applications that a kind of heavy metal has good adsorption effect.
The present invention not only makes full use of the electric property of graphene oxide uniqueness, mechanical property, hot property and high specific area, graphite oxide itself has many carboxyls, the group such as hydroxyl and epoxy radicals, heavy metal has very strong complexing power, and the advantage such as cheap, also the oligomeric 3-aminopropyl triethoxysilane of Promethean employing is interted by electrostatic interaction and graphite oxide and combines, not only can by the expansion of oxidized graphite flake interfloor distance, and amino introducing improves heavy metal adsorption site; The heavy metal absorbent heavy metal obtained has good adsorption effect.
Heavy metal absorbent of the present invention is graphite oxide and oligomeric 3-aminopropyl triethoxysilane compound, and described oligomeric 3-aminopropyl triethoxysilane is got supernatant by 3-aminopropyl triethoxysilane 40 ~ 50 DEG C of hydrolysis and obtained.
Preparation of the present invention is joined in graphite oxide deionization dispersion liquid by oligomeric 3-aminopropyl triethoxysilane deionized water solution, at room temperature stirs, by centrifugal for the flocculent deposit of separating out, and freeze drying and get final product;
Described graphite oxide be standby by Hummers legal system after, be separated through freeze drying and obtain.
3-aminopropyl triethoxysilane hydrolysis time is be advisable for 4 ~ 8 hours.
The concrete embodiment of the present invention is:
Get 3-aminopropyl triethoxysilane mild hydrolysis at 45 DEG C in deionized water, get supernatant, obtain oligomeric 3-aminopropyl triethoxysilane (molecular weight is generally between 196 to 404).Get cryodesiccated graphite oxide through ultrasonic disperse in deionized water.By the 3-aminopropyl triethoxysilane of mild hydrolysis and scattered graphite oxide at room temperature mix and blend.By centrifugal for the flocculent deposit of separating out, moisture is removed in freeze drying can obtain the adsorbent (hereinafter referred to as GN) described in the present invention.
As a comparison, under stirring, the obtained adsorbent of graphite oxide dispersion soln is directly joined (hereinafter referred to as GN by not being hydrolyzed 3-aminopropyl triethoxysilane
0).
Respectively with GN
0be that adsorbent carries out adsorption test to the lead ion of variable concentrations with GN.Absorbent concentration is 1g.L
-1, temperature is 30 DEG C, and adsorption time is 5 hours.Simulation Langmuir adsorption isotherm surveys its adsorbance, obtains GN
0be 151.5mg.g to the adsorbance of lead
-1, and GN is 312.5mg.g to the adsorbance of lead
-1.
Therefore adsorbent in the present invention can be described, and not only preparation method is simple, and heavy metal lead has good removal effect.
Accompanying drawing explanation
Fig. 1. cryodesiccated graphite oxide GO (a) function spend after the scanning electron microscope (SEM) photograph of GN (b).
Fig. 2. the mass spectrogram of oligomeric 3-aminopropyl triethoxysilane.
Fig. 3. adsorbent GN (a) is schemed with the XRD of graphite oxide GO (b).
Detailed description of the invention
Following examples are intended to the present invention instead of limitation of the invention further are described.
Embodiment 1
(1) preparation of graphite oxide
Get the concentrated sulfuric acid of 100mL98%, 2g NaNO
3mixing, slowly adds the KMnO of 4g graphite powder and 12g in ice-water bath
4, add in one hour, mix recession deicing water-bath half an hour, then use boiling water bath, slowly add 180mL intermediate water constant temperature and stir 20 minutes.550mL intermediate water is added in the most backward mixture.With the H of 30%
2o
2consume unreacted KMnO
4.With the abundant purging compound of intermediate water, sulfate radical-free to supernatant.Graphite oxide is put into ultra low temperature freezer freezing, graphite oxide is put into after being frozen into solid and is vacuumized freeze drier and be dried to and remove moisture completely.
(2) graphite oxide-oligomeric 3-aminopropyl triethoxysilane composite preparation
Get the 45 DEG C of hydrolysis 2 hours in 200mL deionized water of 1mL3-aminopropyl triethoxysilane, obtain (molecular weight is between 196 ~ 300) containing the supernatant of oligomeric 3-aminopropyl triethoxysilane.Again with scattered graphite oxide at room temperature mix and blend, by centrifugal for the flocculent deposit of separating out, namely freeze drying obtains the adsorbent GN described in the present invention.
(3) mensuration of GN absorption property
Respectively with GN and GN
0for ABSORBENTS ABSORPTION metallic lead ion carries out adsorption test.The concentration of heavy metal solution is respectively 400mg.L
-1﹑ 300mg.L
-1﹑ 200mg.L
-1﹑ 100mg.L
-1﹑ 70mg.L
-1﹑ 50mg.L
-1and 30mg.L
-1absorbent concentration is 1g.L
-1, temperature is 30 DEG C, and adsorption time is 5 hours.Simulation Langmuir adsorption isotherm surveys its adsorbance.Obtain GN
0be 151.5mg.g to the adsorbance of lead
-1, and GN is 312.5mg.g to the adsorbance of lead
-1.
Embodiment 2
The preparation method of 3-aminopropyl triethoxysilane oligomeric in embodiment 1 is changed into 1mL3-aminopropyl triethoxysilane in 200mL deionized water 45 DEG C hydrolysis 5 hours, obtain the supernatant of the oligomeric 3-aminopropyl triethoxysilane of (molecular weight is in 300 ~ 404 scopes).Other steps are identical with embodiment 1.Simulation Langmuir adsorption isotherm surveys its adsorbance.Obtaining GN to the adsorbance of lead is 300mg.g
-1.
It can thus be appreciated that the adsorption capacity of the GN heavy metal example lead prepared during the molecular weight of oligomeric 3-aminopropyl triethoxysilane is stronger.Because the GN that the GN having the oligomeric amino silicone of small-molecular-weight to prepare is prepared than the oligomeric amino silicone of macromolecule when equal in quality has more amino.
Table 1GN and GN
0to the absorption constant of the Langmuir Isothermal Model that Pb (II) adsorbs
Table 2 heavy metal absorbent of the present invention compares with other sorbing material heavy metal absorption property
Bibliography
[1]Xu Tao,Liu Xiaoqin.Peanut Shell Activated Carbon:Characterization,Surface Modificationand Adsoption of Pb2+from Aqueous solution.Chinese Journal of Chemical Engineering,200816（3）：401-406.
[2]Cao Xinde,Ma L Q,Rhue D R,Appel C S.Mechanisms of lead,copper,and zinc retentionby phosphate rock.Environmental Pollution,2004,131:435-444.
[3]Qu Rongjun,Ji Chunnuan,Sun Yanzhi,Li Zhongfang,Cheng Guoxiang,Song Renfeng.Syntheses and adsorption properties of phenol-formaldehyde-type chelating resins bearing thefunctional group of tartaric acid.Chinese Journal of Polymer Science,2004,22:469-475.
[4]Tang Xin-Hu,Tan Shu-Ying,Wang Yu-Ting.Study of the systhesis of chitosan deivativescontaining benzo-21-crown-7and their adsorpton properties for metal ions.Journal of AppliedPolymer Science,2002,83(9):1886-1891.
Claims (5)
1. a heavy metal absorbent, it is characterized in that, described heavy metal absorbent is graphite oxide and oligomeric 3-aminopropyl triethoxysilane compound, and described oligomeric 3-aminopropyl triethoxysilane is got supernatant by 3-aminopropyl triethoxysilane 40 ~ 50 DEG C of hydrolysis and obtained; Described heavy metal is one or both in plumbous, cadmium.
2., according to a kind of heavy metal absorbent described in claim 1, it is characterized in that, described graphite oxide be standby by Hummers legal system after, be separated through freeze drying and obtain.
3. according to a kind of heavy metal absorbent described in claim 1, it is characterized in that, 3-aminopropyl triethoxysilane hydrolysis time is 2 ~ 8 hours.
4. a preparation method for heavy metal absorbent, is characterized in that, is joined in graphite oxide deionization dispersion liquid by oligomeric 3-aminopropyl triethoxysilane deionized water solution, at room temperature stirs, by centrifugal for the flocculent deposit of separating out, and freeze drying and get final product; Described oligomeric 3-aminopropyl triethoxysilane gets supernatant by 3-aminopropyl triethoxysilane 40 ~ 50 DEG C of hydrolysis to obtain.
5. according to the preparation method described in claim 4, it is characterized in that, 3-aminopropyl triethoxysilane hydrolysis time is 2 ~ 8 hours.
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| JP6053724B2 (en) * | 2014-06-26 | 2016-12-27 | 国立大学法人九州大学 | Ion exchange resin and metal adsorption separation method |
| CN105217716A (en) * | 2015-10-30 | 2016-01-06 | 王立鑫 | Absorbent charcoal composite material of one way of life sewage disposal and preparation method thereof |
| CN105253931A (en) * | 2015-10-30 | 2016-01-20 | 王立鑫 | Activated carbon composite material for increasing industrial wastewater purifying degree and preparation method thereof |
| CN106345466B (en) * | 2016-07-31 | 2020-05-01 | 江苏长三角环境科学技术研究院有限公司 | Preparation method of hydroxylated graphene oxide-magnesium titanate/silver molybdate composite material |
| CN106732383A (en) * | 2016-11-30 | 2017-05-31 | 无锡龙盈环保科技有限公司 | Modified heavy metal in water compound adsorbent of a kind of Graphene and preparation method thereof |
| CN106694037B (en) * | 2016-12-06 | 2019-07-09 | 常州大学 | A kind of catalyst and preparation method thereof for phenol ortho alkylation process |
| CN106824118A (en) * | 2017-03-29 | 2017-06-13 | 邱发龙 | A kind of adsorbent for heavy metal for sewage disposal and preparation method thereof |
| CN107115848A (en) * | 2017-04-26 | 2017-09-01 | 无锡新人居科贸有限公司 | A kind of preparation method and application of heavy metal absorbent |
| CN109529779A (en) * | 2018-11-14 | 2019-03-29 | 常州大学 | A kind of preparation method and applications of modified ZIF-8/GO composite membrane |
| CN109589916A (en) * | 2018-11-29 | 2019-04-09 | 浙江正洁环境科技有限公司 | A kind of heavy metal absorbent and preparation method thereof |
| CN112341579B (en) * | 2020-11-26 | 2023-07-25 | 蚌埠市华东生物科技有限公司 | Adsorption resin for stevioside separation and purification and application thereof |
Citations (1)
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|---|---|---|---|---|
| CN102220036A (en) * | 2011-06-02 | 2011-10-19 | 北京化工大学 | Method for preparing white carbon black modified by silane coupling agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008045599A2 (en) * | 2006-06-16 | 2008-04-17 | World Minerals, Inc. | Heavy metal adsorbent material, processes of making same, and methods of separating heavy metals from fluids |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220036A (en) * | 2011-06-02 | 2011-10-19 | 北京化工大学 | Method for preparing white carbon black modified by silane coupling agent |
Non-Patent Citations (2)
| Title |
|---|
| Preparation and characterization of(3-aminopropyl) triethoxysilane-coated magnetite nanoparticles;M. Yamaura,et al.;《Journal of Magnetism and Magnetic Materials》;20041231;第279卷;第211页左栏第2段、第212页左栏倒数第1段至右栏第2段及附图1和2 * |
| 伍婵翠等.多氨基改性蔗渣对水溶液中Pb2+、Zn2+、Cd2+、Cu2+吸附性能的研究.《材料导报B:研究篇》.2012,第26卷(第6期), * |
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