CN104888686B - A kind of particle red mud base adsorbent preparation method for Phosphate Adsorption - Google Patents

A kind of particle red mud base adsorbent preparation method for Phosphate Adsorption Download PDF

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CN104888686B
CN104888686B CN201510361762.9A CN201510361762A CN104888686B CN 104888686 B CN104888686 B CN 104888686B CN 201510361762 A CN201510361762 A CN 201510361762A CN 104888686 B CN104888686 B CN 104888686B
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red mud
particle
base adsorbent
temperature
neutralization
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CN104888686A (en
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张盼月
叶捷
曾光明
吴彦
张海波
房玮
刘建波
晏铭
苟玺莹
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Hunan University
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Hunan University
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Abstract

The invention discloses a kind of particle red mud base adsorbent preparation method for Phosphate Adsorption, belong to technical field of environmental management.The method includes:The neutralization red mud of acid activation is prepared under certain condition;The neutralization red mud of acid activation, straw powder and hydroxypropyl methyl cellulose are obtained particle red mud base adsorbent under certain condition;The particle red mud base adsorbent that will be prepared is used for phosphatic absorption.The preparation method of particle red mud base adsorbent of the invention is simple and practical, and prepared particle red mud base adsorbent specific surface area is big, with good Phosphate Adsorption ability, is reclaimed for solving red mud pollution and phosphate, realizes that the treatment of wastes with processes of wastes against one another is significant.

Description

A kind of particle red mud base adsorbent preparation method for Phosphate Adsorption
Technical field
The invention belongs to technical field of environmental management, more particularly to a kind of particle red mud base absorption for Phosphate Adsorption Agent preparation method.
Background technology
Red mud is that aluminium industry extracts the contaminative waste residue discharged during aluminum oxide.1 ton of aluminum oxide is often produced, it is average to produce 0.3-2.0 tons of red mud.Annual whole world red mud yield is about 1.2 hundred million tons.Major part red mud relies on the stockyard heap of large area at present Put, still without effective Land use systems, a large amount of soils are not only taken up, serious pollution is also caused to environment.Therefore the money of red mud Sourceization is using extremely urgent.
At present, powder red mud is made adsorbent for phosphatic absorption by existing some researchs.Although separate sources is red The physicochemical property of mud is different, but by having good absorption property to phosphate after appropriate activation.But these powder Last red mud base adsorbent has some limitations in actual applications.Waste water exists by after the treatment of powder red mud base adsorbent The problems such as separation of solid and liquid.If powder red mud base adsorbent is seated in adsorption column carries out Dynamic Adsorption, easily cause adsorption column and block up Plug and the loss of flood peak increase, and absorption is carried out.In order to improve red mud utilizability in practice, granulated be must Right selection.
Powder red mud base adsorbent is granulated research at present is little.In known document, Despland et al. with Red mud powder is neutralized for raw material is prepared for porous particle mud adsorbent.The powder that Yue et al. is produced with burning method aluminium industry Red mud is prepared for particle mud adsorbent for raw material.These relatively low (Phosphate Adsorption amounts of particle mud adsorbent adsorption capacity Less than 10mg/g).Additionally, the patent of invention of Publication No. CN101143312A institute during particle mud adsorbent is prepared Up to 5 kinds of the raw material of use, and need to be calcined by gradient temperature control.The patent of invention of Publication No. CN1317548A with Red mud, flyash, clay are raw material, are equipped with pore creating material and prepare ceramic adsorbent, the ceramic adsorbent intensity and the porosity of preparation Low, absorption property is poor, is not suitable for large-scale popularization and application.Therefore the easy new particle red mud base adsorbent system of exploitation is needed Preparation Method.This patent only prepares particle by raw material of the neutralization red mud of acid activation, hydroxypropyl methyl cellulose and straw powder Red mud base adsorbent, preparation process is simple, with low cost, obtained particle red mud base adsorbent has superior Phosphate Adsorption Performance, can provide a new approaches for the recycling of red mud, with economic, social and environment benefit higher.
The content of the invention
1. goal of the invention
It is an object of the present invention to during overcoming the shortcomings of existing powder red mud absorption phosphate, there is provided a kind of technique Simply, the preparation method of particle red mud base adsorbent that is with low cost, working well.
2. technical scheme
A kind of particle red mud base adsorbent preparation method that the present invention is provided, comprises the following steps:
(1) take a certain amount of original red mud, by its with calcium ions and magnesium ions solution with 1:3-1:5 weight is continuously stirred than mixing Mix until pH reaches 8.2-8.6;
(2) the red mud mixed liquor of above-mentioned addition calcium ions and magnesium ions is carried out into separation of solid and liquid, and uses deionized water rinsing solid-like Solid sample repeatedly, until filtrate pH is in neutrality, is then dried 10-12h by product at a temperature of 100-120 DEG C;
(3) by sieving of being milled after the sample natural cooling after drying, the neutralization that granular size is 100-150 μm is obtained red Mud;
(4) red mud will be neutralized to be added into the hydrochloric acid solution of 8.0-10.0mol/L with the dosage of 0.4-0.5g/L, 4-6h is reacted at a temperature of 40-45 DEG C;
(5) the red mud mixed liquor of above-mentioned addition hydrochloric acid solution is carried out into separation of solid and liquid, and uses deionized water rinsing solid-like Solid sample repeatedly, until filtrate pH is in neutrality, is then dried 10-12h by product at a temperature of 100-120 DEG C;
(6) by sieving of being milled after the sample natural cooling after drying, the acid activation that granular size is 100-150 μm is obtained Neutralize red mud;
(7) straw is dried into 10-12h at a temperature of 100-120 DEG C, sieving of being milled after natural cooling obtains granular size It is 100-150 μm of straw powder;
(8) by the neutralization red mud of acid activation, straw powder and hydroxypropyl methyl cellulose respectively with 82:11:7-71:22:7 Weight than well mixed;
(9) add appropriate deionized water and be sufficiently stirred for rear granulating and forming, particle diameter size is 2-3mm;
(10) by above-mentioned particle in drying at room temperature 24h;
(11) by above-mentioned particle in obtaining particle red mud base adsorbent in 225-250 DEG C of roasting temperature 30-60min.
Particle red mud base adsorbent of the present invention adsorbs phosphatic method, comprises the following steps:
(12) a certain amount of particle red mud base adsorbent is taken, addition initial concentration is for 400-500mg/L, initial soln pH In the phosphate solution of 5-7, the saturated extent of adsorption of particle red mud base adsorbent is determined.
Original red mud in described changed red mud granulating preparation method is bayer process (Bayer process) life Produce remaining slag after aluminum oxide;Straw takes from common farm;Hydroxypropyl methyl cellulose is the commercial product of purchase.
3. beneficial effects of the present invention
(1) the raw material convenient material drawing needed for the present invention, cheap, the preparation method of particle red mud base adsorbent is simply real With with the Technology Potential that heavy industrialization is used;
(2) the particle red mud base adsorbent specific surface area prepared by the present invention is big, with good Phosphate Adsorption ability, Its Phosphate Adsorption amount reaches 69.33-84.56mg/g, has wide utilization prospect in technical field of environmental management;
(3) of the invention this is reclaimed for solving red mud pollution and phosphate, realizes that the treatment of wastes with processes of wastes against one another is significant.
Brief description of the drawings
The surface SEM figures of Fig. 1 particle red mud base adsorbents.
Specific embodiment:
The present invention is expanded on further below by specific embodiment, but is not intended to limit the present invention.
Red mud used is remaining after bayer process (Bayer process) production aluminum oxide in the embodiment of the present invention Slag;Straw takes from common farm;Hydroxypropyl methyl cellulose is the commercial product of purchase.
Embodiment 1:
(1) take a certain amount of original red mud, by its with calcium ions and magnesium ions solution with 1:5 weight is continuously stirred straight than mixing 8.4 are reached to pH;
(2) the red mud mixed liquor of above-mentioned addition calcium ions and magnesium ions is carried out into separation of solid and liquid, and uses deionized water rinsing solid-like Solid sample repeatedly, until filtrate pH is in neutrality, is then dried 12h by product at a temperature of 100 DEG C;
(3) by sieving of being milled after the sample natural cooling after drying, the neutralization red mud that granular size is 100 μm is obtained;
(4) red mud will be neutralized to be added into the hydrochloric acid solution of 10.0mol/L with the dosage of 0.5g/L, at a temperature of 40 DEG C Reaction 5h;
(5) the red mud mixed liquor of above-mentioned addition hydrochloric acid solution is carried out into separation of solid and liquid, and uses deionized water rinsing solid-like Solid sample repeatedly, until filtrate pH is in neutrality, is then dried 12h by product at a temperature of 100 DEG C;
(6) by sieving of being milled after the sample natural cooling after drying, the neutralization of the acid activation that granular size is 100 μm is obtained Red mud;
(7) straw is dried into 12h at a temperature of 100 DEG C, sieving of being milled after natural cooling obtains granular size for 100 μm Straw powder;
(8) by the neutralization red mud of acid activation, straw powder and hydroxypropyl methyl cellulose respectively with 71:22:7 weight ratio It is well mixed;
(9) add appropriate deionized water and be sufficiently stirred for rear granulating and forming, particle diameter size is 2mm;
(10) by above-mentioned particle in drying at room temperature 24h;
(11) by above-mentioned particle in obtaining particle red mud base adsorbent in 225 DEG C of roasting temperature 30min.
The particle red mud base adsorbent prepared with embodiment 1 carries out the Phosphate Adsorption of example 2 below.
Embodiment 2:
Preparation initial concentration is 500mg/L, and initial pH value is 7.0 phosphate solution, the red mud for adding embodiment 1 to prepare Particle, under 40 DEG C of temperature conditionss, 48h is stirred with the rotating speed of 100rpm.Acquired results are as follows:The specific surface area of red mud particle And total hole volume is respectively 113.54m2/ g and 0.0287cm3/g.The Phosphate Adsorption amount of unit grain red mud base adsorbent reaches 84.56mg/g.
Embodiment 3:
(1) take a certain amount of original red mud, by its with calcium ions and magnesium ions solution with 1:5 weight is continuously stirred straight than mixing 8.4 are reached to pH;
(2) the red mud mixed liquor of above-mentioned addition calcium ions and magnesium ions is carried out into separation of solid and liquid, and uses deionized water rinsing solid-like Solid sample repeatedly, until filtrate pH is in neutrality, is then dried 12h by product at a temperature of 100 DEG C;
(3) by sieving of being milled after the sample natural cooling after drying, the neutralization red mud that granular size is 100 μm is obtained;
(4) red mud will be neutralized to be added into the hydrochloric acid solution of 10.0mol/L with the dosage of 0.5g/L, at a temperature of 40 DEG C Reaction 5h;
(5) the red mud mixed liquor of above-mentioned addition hydrochloric acid solution is carried out into separation of solid and liquid, and uses deionized water rinsing solid-like Solid sample repeatedly, until filtrate pH is in neutrality, is then dried 12h by product at a temperature of 100 DEG C;
(6) by sieving of being milled after the sample natural cooling after drying, the neutralization of the acid activation that granular size is 100 μm is obtained Red mud;
(7) straw is dried into 12h at a temperature of 100 DEG C, sieving of being milled after natural cooling obtains granular size for 100 μm Straw powder;
(8) by the neutralization red mud of acid activation, straw powder and hydroxypropyl methyl cellulose respectively with 81:11:7 weight ratio It is well mixed;
(9) add appropriate deionized water and be sufficiently stirred for rear granulating and forming, granular size is 2mm;
(10) by above-mentioned particle in drying at room temperature 24h;
(11) by above-mentioned particle in obtaining particle red mud base adsorbent in 250 DEG C of roasting temperature 30min.
The particle red mud prepared with embodiment 3 carries out the Phosphate Adsorption of example 4 below.
Embodiment 4:
Preparation initial concentration is 500mg/L, and initial pH value is 7.0 phosphate solution, the red mud for adding embodiment 1 to prepare Particle, under 20 DEG C of temperature conditionss, 48h is stirred with the rotating speed of 100rpm.Acquired results are as follows:The specific surface area of red mud particle And total hole volume is respectively 90.70m2/ g and 0.0104cm3/g.The Phosphate Adsorption amount of unit grain red mud base adsorbent reaches 69.33mg/g。

Claims (1)

1. a kind of preparation method of particle red mud base adsorbent, it is characterised in that the described method comprises the following steps:Take a certain amount of Bayer process (Bayer process) production aluminum oxide after remaining slag as original red mud, by itself and calcium ions and magnesium ions Solution is with 1:3-1:5 weight is continuously stirred until pH reaches 8.2-8.6 than mixing, then carries out separation of solid and liquid, and spend from Sub- water rinses solid sample repeatedly, until filtrate pH is in neutrality, solid sample is then dried into 10- at a temperature of 100-120 DEG C 12h;By sieving of being milled after the sample natural cooling of drying, the neutralization red mud that granular size is 100-150 μm is obtained;In 40-45 Under the conditions of DEG C, above-mentioned neutralization red mud is added in 8.0-10.0mol/L hydrochloric acid solutions carries out priming reaction 4-6h, and is consolidated Liquid is separated, and, until filtrate pH is in neutrality, then by solid sample in 100-120. with deionized water rinsing solid sample repeatedly 10-12h is dried at a temperature of DEG C;By sieving of being milled after the sample natural cooling of drying, the acid that granular size is 100-150 μm is obtained The neutralization red mud of activation;Straw is dried into 10-12h at a temperature of 100-120 DEG C, sieving of being milled after natural cooling obtains particle Size is 100-150 μm of straw powder;By 100-150 μm of acid activation neutralize red mud, 100-150 μm of straw powder and Hydroxypropyl methyl cellulose presses 82:11:7-71:22:7 ratios are well mixed, and after adding appropriate deionized water to be sufficiently stirred for Granulating and forming, particle diameter size is 2-3mm;The particle that will be obtained is under drying at room temperature 24h, 225-250 DEG C of temperature conditionss Roasting 30-60min, obtains particle red mud base adsorbent.
CN201510361762.9A 2015-06-26 2015-06-26 A kind of particle red mud base adsorbent preparation method for Phosphate Adsorption Expired - Fee Related CN104888686B (en)

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CN113634222A (en) * 2021-08-20 2021-11-12 中国人民大学 Red mud ceramsite adsorbent and preparation method and application thereof
CN115138336B (en) * 2022-06-29 2023-07-18 北京科技大学 Preparation method of red mud-peanut shell-based composite material for treating acidic phosphorus-containing sewage
CN116492978B (en) * 2023-05-05 2024-02-09 陕西科技大学 Zn 2+ Modified industryZAS/GRM composite material of waste red mud, and preparation method and application thereof

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CN104072189B (en) * 2014-07-08 2015-10-07 尹小林 The method of light porous agglomerated material is manufactured with red mud and plant residue

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