CN102167371B - Preparation method of modified magnalium binary hydrotalcites and application of modified magnalium binary hydrotalcites in absorbing bisphenol A in water body - Google Patents

Preparation method of modified magnalium binary hydrotalcites and application of modified magnalium binary hydrotalcites in absorbing bisphenol A in water body Download PDF

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CN102167371B
CN102167371B CN 201110008900 CN201110008900A CN102167371B CN 102167371 B CN102167371 B CN 102167371B CN 201110008900 CN201110008900 CN 201110008900 CN 201110008900 A CN201110008900 A CN 201110008900A CN 102167371 B CN102167371 B CN 102167371B
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houghite
hydrotalcites
binary
magnalium
magnalium binary
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CN102167371A (en
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李燕
毕浩宇
毛晓明
臧运波
周成勇
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Changzhi University
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Changzhi University
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Abstract

The invention belongs to the technical field of hydrotalcites, in particular relating to a preparation method of modified magnalium binary hydrotalcites and application of the modified magnalium binary hydrotalcites in absorbing bisphenol A in water body, aiming at solving the technical problems that the adsorbent is difficulty in regeneration, high in cost and the like since the bisphenol A in the waste water is absorbed and treated by the adsorbent such as the active carbon, the macroporous absorption resin and the like in the prior art. The preparation method of the modified magnalium binary hydrotalcites comprises the following steps: roasting the magnalium binary hydrotalcites at a temperature of 400-500 DEG C for 4-7 hours to obtain magnalium thermometal oxide, dissolving the obtained magnalium thermometal oxide into a lauryl sodium sulfate solution according to 100% of ion exchange capacity, adjusting the PH value to 9-10 by utilizing a NaOH solution, stirring for 42-54 hours in the presence of N2, filtering, washing, precipitating, and baking at the temperature of 55-65 DEG C until the weight is constant so as to obtain the modified magnalium binary hydrotalcites. The invention has the advantages that the hydrotalcites are reproduceable, the cost is low and the like.

Description

A kind of preparation method of modification magnalium binary houghite and the application of dihydroxyphenyl propane in the adsorption treatment water body thereof
Technical field
The invention belongs to the hydrotalcite technical field, be specifically related to a kind of preparation method of modification magnalium binary houghite and the application of dihydroxyphenyl propane in the adsorption treatment water body.
Background technology
Dihydroxyphenyl propane (BPA), chemical name is the 4-dihydroxy-diphenyl propane, important chemical substance in the Plastic Resin products production and important fine chemical material, be widely used in industry and homebrew, dihydroxyphenyl propane also is a kind of endocrine disrupter simultaneously, endocrine system to animal and human's body has certain influence, and because dihydroxyphenyl propane has obvious lipotropy, easily enrichment in aquatic organism, therefore in municipal effluent, trade effluent, mud, soil, river, earth's surface and percolate, all be enriched with dihydroxyphenyl propane, threatening the health of people and organism.Therefore, it is significant to the reparation of sewage disposal and contaminated soil to seek a kind of efficient dihydroxyphenyl propane treatment agent.
Domestic and international treatment process for dihydroxyphenyl propane in the water body adopts absorption method more at present, and sorbent material commonly used has gac, macroporous adsorbent resin etc., although wherein charcoal absorption adsorptive capacity is large, and the regeneration difficulty, thereby it uses good as people gradually; Desorb is easy, adsorption rate is high and the selectivity high though macroporous resin has, and its cost is higher, has directly affected applying of it.
The oxyhydroxide with hydrotalcite layered structure that houghite compound (being called for short HTlc) is comprised of divalent-metal ion and trivalent metal ion.Chemical general formula is: [M 2+ 1-xM 3+ x(OH) 2] X+(A N- X/n) X-MH 2O, wherein M 2+Represent divalent-metal ion, such as Mg 2+, Mn 2+, Fe 2+, Co 2+, Zn 2+, Cu 2+Deng; M 3+Represent trivalent metal ion, such as Al 3+, Cr 3+, Fe 3+, Sc 3+, V 3+Deng; A refers to that valence mumber is-negatively charged ion of n; X refers to M among every mole of HTlc 3+Mole number; M is the mole number of crystal water in every mole of houghite, and houghite compound has larger specific surface area through after the roasting, is usually used in some negatively charged ion waste water of adsorption treatment.The houghite of surface modification (as modifying with anion surfactant), that is modification houghite, make the houghite interlayer form hydrophobic region, the interlayer channel height is increased, can be used as the sorbent material of hydrophobic organic compound, but yet there are no modification magnalium binary houghite for the application in the adsorption treatment aqueous systems dihydroxyphenyl propane.
Summary of the invention
Main purpose of the present invention is to have dihydroxyphenyl propane in the sorbent material adsorption treatment waste water such as gac, macroporous adsorbent resin to have adsorbent reactivation difficulty, cost high-technology problem for available technology adopting, the preparation method of the modification magnalium binary houghite that provide a kind of and reuse, cost is low and the application of dihydroxyphenyl propane in the adsorption treatment water body thereof.
The preparation method of modification magnalium binary houghite of the present invention is: the magnalium binary houghite was obtained the magnalium bimetallic oxide in 4~7 hours in 400~500 ℃ of roastings, be dissolved in the lauryl sodium sulfate aqueous solution by 100% ion exchange capacity, regulating the pH value with NaOH solution is 9~10, at N 2Protection is lower stirred 42~54 hours, and then filtration, washing precipitation dry to constant weight at 55~65 ℃, obtain modification magnalium binary houghite;
Wherein said magnalium binary houghite general formula is: [Mg 2+ 1-xAl 3+ x(OH) 2] (Cl -) xMH 2O, in the formula, x is Al 3+/ (Mg 2++ Al 3+) the ratio of amount of substance, 0.2<x<0.4, m is interlayer crystal water mole number in every mole of houghite, 2<m<6.
Wherein the preferred magnalium binary houghite of the present invention chemical formula is: [Mg 2+ 0.68Al 3+ 0.32(OH) 2] (Cl -) 0.323H 2O.
The application of modification magnalium binary houghite of the present invention dihydroxyphenyl propane in the adsorption treatment water body, modification magnalium binary houghite input is contained in the water body of dihydroxyphenyl propane, adding sodium-chlor concentration of sodium-chlor to the water is 0.01~0.1mol/L, regulating water pH value is 6~10, carries out adsorption treatment and got final product in 1~24 hour under 25~45 ℃.
Recovery method after modification magnalium binary houghite uses: the modification magnalium binary houghite that will adsorb behind the dihydroxyphenyl propane places dehydrated alcohol, and 20~30 ℃ vibrated 1~2 hour, reclaimed throw out behind the high speed centrifugation, and drying to constant weight at 55-65 ℃ obtains.
Modification magnalium binary houghite synthetic method of the present invention is simple, and the increase of the magnalium binary houghite interlayer channel height after the modification, has increased its absorption property; Because modification magnalium binary houghite is water insoluble, can not cause secondary pollution to water body after the use, recovery method is also very simple; Magnalium binary houghite cost is lowered into the expense of sewage disposal well below the macroporous adsorbent resin material.
Embodiment
Embodiment 1:
The preparation method of modification magnalium binary houghite: with binary magnesium-aluminum hydrotalcite [Mg 2+ 0.68Al 3+ 0.32(OH) 2] (Cl -) 0.323H 2O made the magnalium bimetallic oxide in 4 hours in 400 ℃ of roastings, was dissolved in the lauryl sodium sulfate aqueous solution by 100% ion exchange capacity, and regulating the pH value with the NaOH of 0.01mol/L is 9, at N 2Protection is lower stirred 42 hours, and then filtration, washing precipitation dry to constant weight at 55 ℃, make the modification binary magnesium-aluminum hydrotalcite.
The application of modification magnalium binary houghite dihydroxyphenyl propane in the adsorption treatment water body of present embodiment preparation: the above-mentioned modification binary magnesium-aluminum hydrotalcite input that makes is contained in the water body of dihydroxyphenyl propane, adding sodium-chlor concentration of sodium-chlor to the water is 0.01mol/L, regulating water pH value is 6, carries out adsorption treatment and got final product in 1 hour under 25 ℃.
Embodiment 2:
The preparation method of modification magnalium binary houghite: with magnalium binary houghite [Mg 2+ 0.65Al 3+ 0.35(OH) 2] (Cl -) 0.352.7H 2O made the magnalium bimetallic oxide in 5 hours in 450 ℃ of roastings, was dissolved in the lauryl sodium sulfate aqueous solution by 100% ion exchange capacity, and regulating the pH value with the NaOH of 0.01mol/L is 9.5, at N 2Protection is lower stirred 48 hours, and then filtration, washing precipitation dry to constant weight at 60 ℃, make modification magnalium binary houghite.
The application of modification magnalium binary houghite dihydroxyphenyl propane in the adsorption treatment water body of present embodiment preparation: the above-mentioned modification magnalium binary houghite input that makes is contained in the water body of dihydroxyphenyl propane, adding sodium-chlor concentration of sodium-chlor to the water is 0.05mol/L, regulating water pH value is 8, carries out adsorption treatment and got final product in 10 hours under 35 ℃.
Embodiment 3:
The preparation method of present embodiment modification magnalium binary houghite is: with magnalium binary houghite [Mg 2+ 0.67Al 3+ 0.33(OH) 2] (Cl -) 0.332.9H 2O made the magnalium bimetallic oxide in 7 hours in 500 ℃ of roastings, was dissolved in the lauryl sodium sulfate aqueous solution by 100% ion exchange capacity, and regulating the pH value with the NaOH of 0.01mol/L is 10, at N 2Protection is lower stirred 54 hours, and then filtration, washing precipitation dry to constant weight at 65 ℃, make modification magnalium binary houghite.
The application of modification magnalium binary houghite dihydroxyphenyl propane in the adsorption treatment water body of present embodiment preparation: the above-mentioned modification magnalium binary houghite input that makes is contained in the water body of dihydroxyphenyl propane, adding sodium-chlor concentration of sodium-chlor to the water is 0.1mol/L, regulating water pH value is 10, carries out adsorption treatment and got final product in 24 hours under 45 ℃.

Claims (2)

1. the application of modification magnalium binary houghite dihydroxyphenyl propane in the adsorption treatment water body, it is characterized in that: modification magnalium binary houghite is dropped into contain in the water body of dihydroxyphenyl propane, adding sodium-chlor concentration of sodium-chlor to the water is 0.01 ~ 0.1mol/L, regulating water pH value is 6 ~ 10, carries out adsorption treatment and got final product in 1 ~ 24 hour under 25 ~ 45 ° of C;
Wherein said magnalium binary houghite general formula is: [Mg 2+ 1-xAl 3+ x(OH) 2] (Cl -) xMH 2O, in the formula, x is Al 3+/ (Mg 2++ Al 3+) the ratio of amount of substance, 0.2<x<0.4, m is interlayer crystal water mole number in every mole of houghite, 2<m<6; Concrete preparation method is: the magnalium binary houghite was obtained the magnalium bimetallic oxide in 4 ~ 7 hours in 400 ~ 500 ° of C roastings, be dissolved in the lauryl sodium sulfate aqueous solution by 100% ion exchange capacity, regulating the pH value with NaOH solution is 9~10, at N 2Protection is lower stirred 42 ~ 54 hours, and then filtration, washing precipitation dry to constant weight at 55 ~ 65 ℃, obtain modification magnalium binary houghite.
2. the application of modification magnalium binary houghite according to claim 1 dihydroxyphenyl propane in the adsorption treatment water body, it is characterized in that: described magnalium binary houghite chemical formula is: [Mg 2+ 0.68Al 3+ 0.32(OH) 2] (Cl -) 0.323H 2O.
CN 201110008900 2011-01-11 2011-01-11 Preparation method of modified magnalium binary hydrotalcites and application of modified magnalium binary hydrotalcites in absorbing bisphenol A in water body Expired - Fee Related CN102167371B (en)

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CN102872809B (en) * 2012-09-20 2014-04-30 常州大学 Organic hydrotalcite and preparation method thereof
CN105080550B (en) * 2015-06-03 2018-01-12 博天环境集团股份有限公司 The preparation method of the ozone oxidation catalyst of gas treatment waste water
CN106179228A (en) * 2016-09-01 2016-12-07 桂林理工大学 A kind of preparation method of bagasse charcoal/magnesium aluminum-hydrotalcite compound adsorbent
CN106311138A (en) * 2016-09-01 2017-01-11 桂林理工大学 Preparation method of bagasse charcoal and magnesium-iron hydrotalcite composite adsorbent
CN106928042A (en) * 2017-04-14 2017-07-07 华中农业大学 A kind of method of Solid phase extraction separation gossypol in solution from gossypol
CN107469861B (en) * 2017-08-30 2020-09-04 江南大学 Ir @ Cu @ BINAL @ HT catalyst for bisphenol F synthesis and preparation method
CN109701578A (en) * 2019-01-16 2019-05-03 山西大学 A kind of preparation method and applications of copper aluminium houghite/nitrating carbon fiber composite catalyst
CN112657470A (en) * 2020-12-03 2021-04-16 乌日娜 Method for modifying hydrotalcite by using long carbon chain anionic surfactant
CN113318702B (en) * 2021-04-09 2022-10-11 吉林化工学院 Preparation and application of modified bimetal oxide
CN114984991A (en) * 2022-05-24 2022-09-02 浙江微通催化新材料有限公司 g-C 3 N 4 Preparation method of modified hydrotalcite catalyst and application of modified hydrotalcite catalyst in condensation reaction of furfural and cyclic ketone

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