CN103143325A - Preparation method of glutamic acid intercalated layer hydrotalcite heavy-metal adsorbent - Google Patents
Preparation method of glutamic acid intercalated layer hydrotalcite heavy-metal adsorbent Download PDFInfo
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- CN103143325A CN103143325A CN2013100888738A CN201310088873A CN103143325A CN 103143325 A CN103143325 A CN 103143325A CN 2013100888738 A CN2013100888738 A CN 2013100888738A CN 201310088873 A CN201310088873 A CN 201310088873A CN 103143325 A CN103143325 A CN 103143325A
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Abstract
The invention relates to a preparation method of a glutamic acid intercalated layer hydrotalcite heavy-metal adsorbent, and discloses a preparation method of a metal adsorbent. The method comprises the following steps of: (1) preparing magnesium nitrate and aluminum nitrate salt solutions and a sodium hydroxide alkali solution; (2) dissolving glutamic acid or tartaric acid into CO2-eliminating deionized water, and preparing an acid solution; (3) simultaneously dripping the metal salt solutions and the alkali solution to the acid solution at room temperature under the protection of N2, and controlling the pH to be in a range of 9-10; and (4) crystallizing slurry obtained after the dripping is finished at 60 DEG C under the protection of N2 for 12 hours, and then filtering, washing and drying to obtain a product. The glutamic acid intercalated layer hydrotalcite prepared through the method disclosed by the invention can be used for fast absorbing the Pb<2+> ions contained in water.
Description
Technical field
The present invention relates to the preparation method of attached dose an of metal ion species, particularly relate to a kind of preparation method of glutamic acid intercalated hydrotalcite heavy metal absorbent.
Background technology
In a single day the heavy metal ion that exists in underground water, drinking water and waste water reaches certain concentration will harm humans, livestock and aquatic environment.The method of separation and recovery heavy metal mainly comprises chemical precipitation method, membrane separation process, solvent extraction, absorption method etc.The relative additive method of absorption method has the many advantages such as environmental pollution is little, the rate of adsorption is fast, adsorbent is renewable, regenerability is good, in especially processing, low concentration wastewater is respond well.The many kinds of solids material can be used as adsorbent, fiber as useless in active carbon, zeolite, clay, agricultural or forest, ion exchange resin, biomaterial etc.
In recent years, layered di-hydroxyl composite metal oxidate (LDHs) claims again houghite compound (HTLCs) or anionic clay, because its stronger ion-exchange capacity has been subject to paying close attention to widely.Hydrotalcite is comprised of positively charged laminate and interlayer anion, and interlayer anion can be replaced by other anion isomorphous, so hydrotalcite can be used as the organic and inorganic ion that high-efficiency adsorbent is used for removing waste water.
Zhao etc. adopt MgAl-CO
3Pb in the hydrotalcite adsorbed water
2+Obtained adsorption effect preferably, the anion intercalated hydrotalcite of the discovery EDTA such as Kameda can be rapidly and selectively absorb Cu from the aqueous solution
2+, Cd
2+, Pb
2+And Cd
2+Plasma, this is owing to having formed the reason of EDTA-metallo-chelate at the LDH interlayer.Other chelating agents such as citric acid, malic acid and tartaric acid were also once attempted introducing the magnalium hydrotalcite interlayer, were used for absorbing the Cu in water
2+And Cd
2+Plasma.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of glutamic acid intercalated hydrotalcite heavy metal absorbent, the method is take magnesium nitrate, aluminum nitrate, glutamic acid and NaOH as raw material, adopt preparation glutamic acid intercalated hydrotalcite under the low basicity of coprecipitation, it is removed lead ion successful in water as adsorbent.
The objective of the invention is to be achieved through the following technical solutions:
A kind of preparation method of glutamic acid intercalated hydrotalcite heavy metal absorbent, the preparation process of glutamic acid intercalated hydrotalcite heavy metal absorbent comprises:
(1) salting liquid of preparation magnesium nitrate, aluminum nitrate, wherein the Mg/Al mol ratio is 2 or 3, and total concentration of metal ions is 1M;
(2) preparation glutamic acid acid solution, the mole of glutamic acid is Al
3+2 times;
(3) sodium hydroxide solution of preparation 0.5M;
(3) room temperature N
2Under protection, metal salt solution and aqueous slkali are added drop-wise in acid solution simultaneously, control pH=9 ~ 10;
(4) drip 60 ℃, slurries, the N that obtains after end
2The lower crystallization of protection 12 hours is filtered afterwards, is washed, drying, namely gets product.
Advantage of the present invention and effect are:
The present invention adopts preparation glutamic acid intercalated hydrotalcite under the low basicity of coprecipitation take magnesium nitrate, aluminum nitrate, glutamic acid and NaOH as raw material.Glutamic acid is a kind of biodegradable chelating agent that is easy to, and is cheap and easy to get, the magnalium hydrotalcite of preparation glutamic acid intercalated, the Pb in glutamic acid intercalated hydrotalcite energy quick adsorption water
2+, Cu
2+, Cr
6+Ion utilizes this method to make Pb in glutamic acid intercalated hydrotalcite adsorbed water
2+, Cu
2+, Cr
6+Ion has good adsorption effect.
Description of drawings
Fig. 1 is the XRD spectra of glutamic acid intercalated hydrotalcite;
Fig. 2 is the SEM figure of glutamic acid intercalated hydrotalcite;
Fig. 3 is Different L DH/Pb
2+Pb under proportioning
2+Clearance;
Fig. 4 is different Pb
2+Pb under initial concentration
2+Adsorption rate;
Fig. 5 be different Mg/Al than hydrotalcite to Pb
2+The comparison diagram of clearance.
Annotate: accompanying drawing of the present invention is analysis schematic diagram or the photo (only for reference) of product state, the unintelligible understanding that does not affect technical solution of the present invention of figure Chinese word or image.
The specific embodiment
The present invention is described in detail below in conjunction with embodiment.
Embodiment 1
(1) salting liquid of preparation magnesium nitrate, aluminum nitrate, wherein the Mg/Al mol ratio is 2, and total concentration of metal ions is 1M;
(2) sodium hydroxide solution of preparation 0.5M;
(3) room temperature N
2Under protection, metal salt solution and aqueous slkali are added drop-wise in acid solution simultaneously, control pH=9 ~ 10;
(4) drip 60 ℃, slurries, the N that obtains after end
2The lower crystallization of protection 12 hours is filtered afterwards, is washed, drying, namely gets product.The XRD spectra and the surface topography that make hydrotalcite are seen accompanying drawing 1,2.
Under 25 ℃, Mg-Al-G LDH sample is joined and contain Pb
2+In solution, in order to prevent forming the lead hydroxide precipitation, be 0.1molL with concentration in experimentation
-1HNO
3PH is adjusted to 5.0.N in operating process
2Enter in solution with the bubbling form.Press different time interval taking-up sample, pass through fast the membrane filtration of 0.45 μ m.Use spectrophotometric determination Pb
2+Concentration.
At Pb
2+Initial concentration be under the condition of 100 mg/L, Different L DH/Pb
2+Pb under proportioning
2+Adsorption rate the results are shown in accompanying drawing 3.After test result shows 30 min, absorption reaches balance substantially, and speed is very fast.Along with LDH/Pb
2+Increase Pb
2+Clearance increases gradually.But, take into account the expense of practical application, LDH/Pb
2+Proportioning is advisable with 2:1.
At LDH/ Pb
2+=3:1, different Pb
2+Pb under initial concentration
2+Adsorption rate the results are shown in accompanying drawing 4.Result shows: be the Pb of 80 mg/L for initial concentration
2+Liquid to be measured through 30 min after, substantially reach balance, clearance can reach 92.3 %, when initial concentration increased to 130 mg/L, corresponding clearance was reduced to 85.4 %, and initial concentration is when being 150 mg/L, Pb under similarity condition
2+Clearance only reaches 60.3%, visible Pb
2+Initial concentration is lower, and clearance is higher.
Embodiment 2
Preparation Mg/Al mol ratio is 3 magnesium nitrate, the salting liquid of aluminum nitrate, and wherein total concentration of metal ions is 1M, and all the other steps are with embodiment 1.
Adopt LDH/Pb (II)=1:1, Pb
2+Under the condition of initial concentration 100 mg/L, the hydrotalcite of preparation is to Pb
2+Remove capability result and see accompanying drawing 5.Experimental result shows: Mg/Al is not so good as Mg/Al than being the hydrotalcite of 2:1 than the hydrotalcite removal effect for 3:1, and the hydrotalcite of low Mg/Al ratio is to Pb
2+Removal effect good.
Claims (1)
1. the preparation method of a glutamic acid intercalated hydrotalcite heavy metal absorbent, is characterized in that, the preparation process of described glutamic acid intercalated hydrotalcite heavy metal absorbent comprises:
(1) salting liquid of preparation magnesium nitrate, aluminum nitrate, wherein the Mg/Al mol ratio is 2 or 3, and total concentration of metal ions is 1M;
(2) preparation glutamic acid acid solution, the mole of glutamic acid is Al
3+2 times;
(3) sodium hydroxide solution of preparation 0.5M;
(3) room temperature N
2Under protection, metal salt solution and aqueous slkali are added drop-wise in acid solution simultaneously, control pH=9 ~ 10;
(4) drip 60 ℃, slurries, the N that obtains after end
2The lower crystallization of protection 12 hours is filtered afterwards, is washed, drying, namely gets product.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104324693A (en) * | 2014-11-03 | 2015-02-04 | 广东电网有限责任公司电力科学研究院 | Layered composite material with selective water adsorption property and preparation method and application thereof |
| CN105854811A (en) * | 2016-04-05 | 2016-08-17 | 济南大学 | Preparation of sodium alginate intercalated hydrotalcite adsorbent and application thereof |
| CN106044928A (en) * | 2016-07-22 | 2016-10-26 | 东北林业大学 | Intercalated hydrotalcite based composite material with lignosulfonic acid radicals, method for preparing intercalated hydrotalcite based composite material and application thereof |
| CN106881067A (en) * | 2017-04-24 | 2017-06-23 | 北京化工大学 | A kind of modified houghite adsorbent and its application |
| CN107236305A (en) * | 2017-07-07 | 2017-10-10 | 东莞市联洲知识产权运营管理有限公司 | A kind of fire-resisting cable silicon rubber composite material and preparation method thereof |
| CN108144577A (en) * | 2017-12-06 | 2018-06-12 | 常州杰轩纺织科技有限公司 | A kind of preparation method of heavy metal ion adsorbing material |
| CN108176348A (en) * | 2017-12-01 | 2018-06-19 | 谢新昇 | A kind of preparation method of houghite vegetable oil adsorption deacidification agent |
| CN108585630A (en) * | 2018-05-18 | 2018-09-28 | 赵顺全 | A kind of preparation method of high intensity moisture absorption mineral wool board |
| CN109847786A (en) * | 2019-03-06 | 2019-06-07 | 常州大学 | A kind of preparation method and application of Z-type photochemical catalyst MgAlLDH/CN-H |
| CN110624513A (en) * | 2019-10-09 | 2019-12-31 | 武汉纺织大学 | Polyaspartic acid intercalated hydrotalcite composite material and preparation method and application thereof |
| CN111117452A (en) * | 2019-12-27 | 2020-05-08 | 深圳市唯特偶新材料股份有限公司 | Nano environment-friendly low-odor heat-conducting three-proofing paint |
| CN114307999A (en) * | 2021-12-30 | 2022-04-12 | 重庆大学 | Preparation method and application of lysine modified hydrotalcite-like adsorption material |
-
2013
- 2013-03-20 CN CN201310088873.8A patent/CN103143325B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
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| 杨金田等: "谷氨酸插层镁铝水滑石微观结构与性能:实验与理论研究", 《矿物学报》 * |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104324693A (en) * | 2014-11-03 | 2015-02-04 | 广东电网有限责任公司电力科学研究院 | Layered composite material with selective water adsorption property and preparation method and application thereof |
| CN105854811A (en) * | 2016-04-05 | 2016-08-17 | 济南大学 | Preparation of sodium alginate intercalated hydrotalcite adsorbent and application thereof |
| CN106044928A (en) * | 2016-07-22 | 2016-10-26 | 东北林业大学 | Intercalated hydrotalcite based composite material with lignosulfonic acid radicals, method for preparing intercalated hydrotalcite based composite material and application thereof |
| CN106881067B (en) * | 2017-04-24 | 2019-08-02 | 北京化工大学 | A kind of modified houghite adsorbent and its application |
| CN106881067A (en) * | 2017-04-24 | 2017-06-23 | 北京化工大学 | A kind of modified houghite adsorbent and its application |
| CN107236305A (en) * | 2017-07-07 | 2017-10-10 | 东莞市联洲知识产权运营管理有限公司 | A kind of fire-resisting cable silicon rubber composite material and preparation method thereof |
| CN108176348A (en) * | 2017-12-01 | 2018-06-19 | 谢新昇 | A kind of preparation method of houghite vegetable oil adsorption deacidification agent |
| CN108144577A (en) * | 2017-12-06 | 2018-06-12 | 常州杰轩纺织科技有限公司 | A kind of preparation method of heavy metal ion adsorbing material |
| CN108585630A (en) * | 2018-05-18 | 2018-09-28 | 赵顺全 | A kind of preparation method of high intensity moisture absorption mineral wool board |
| CN108585630B (en) * | 2018-05-18 | 2021-05-25 | 陈露 | Preparation method of high-strength moisture-absorption mineral wool board |
| CN109847786A (en) * | 2019-03-06 | 2019-06-07 | 常州大学 | A kind of preparation method and application of Z-type photochemical catalyst MgAlLDH/CN-H |
| CN109847786B (en) * | 2019-03-06 | 2021-12-21 | 常州大学 | Preparation method and application of Z-type photocatalyst MgAlLDH/CN-H |
| CN110624513A (en) * | 2019-10-09 | 2019-12-31 | 武汉纺织大学 | Polyaspartic acid intercalated hydrotalcite composite material and preparation method and application thereof |
| CN111117452A (en) * | 2019-12-27 | 2020-05-08 | 深圳市唯特偶新材料股份有限公司 | Nano environment-friendly low-odor heat-conducting three-proofing paint |
| CN114307999A (en) * | 2021-12-30 | 2022-04-12 | 重庆大学 | Preparation method and application of lysine modified hydrotalcite-like adsorption material |
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|---|---|
| CN103143325B (en) | 2014-12-10 |
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