CN102249277B - Method for deironing aluminum chloride solution - Google Patents

Method for deironing aluminum chloride solution Download PDF

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Publication number
CN102249277B
CN102249277B CN 201110104081 CN201110104081A CN102249277B CN 102249277 B CN102249277 B CN 102249277B CN 201110104081 CN201110104081 CN 201110104081 CN 201110104081 A CN201110104081 A CN 201110104081A CN 102249277 B CN102249277 B CN 102249277B
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Prior art keywords
resin
hydrochloric acid
aluminum chloride
liquor alumini
alumini chloridi
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CN102249277A (en
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郭昭华
吕子剑
蒋引珊
魏存弟
李楠
李晓兵
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China Shenhua Energy Co Ltd
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China Shenhua Energy Co Ltd
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  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Treatment Of Water By Ion Exchange (AREA)

Abstract

The invention relates to a method for deironing aluminum chloride solution, which comprises the following steps of: introducing iron-containing aluminum chloride solution into a resin column, and deironing by using the iron adsorption capacity of resin to obtain aluminum chloride refined solution, wherein the pH value of the aluminum chloride solution is 1.0 to 3.0, the processing temperature is room temperature to 90 DEG C, and the flow rate is the aluminum chloride solution in an amount which is 1 to 4 times the volume of the resin per hour. The method has the characteristics that the process is simple, the production process is easy to control, and product quality is stable. In addition, by the method, the raw material source of low-iron aluminum chloride solution and a subsequent product thereof can be expanded, and production cost is reduced.

Description

A kind of method of removing iron from solution of aluminum chloride
Technical field
The present invention relates to a kind of method of removing iron from solution of aluminum chloride, be specifically related to a kind of method that adopts resins exchange is carried out deep iron removal to liquor alumini chloridi method.
Background technology
Liquor alumini chloridi is the important liquid starting material of the products such as preparation polymerize aluminum chloride, aluminium chlorohydroxide and crystal aluminum chloride.Liquor alumini chloridi is in production or storage and transport process, because the pollution of material purity deficiency or pipeline, container contains a certain amount of iron sometimes.These iron exist in solution with the form of ion.In the process of the products such as preparation polymerize aluminum chloride, aluminium chlorohydroxide or crystal aluminum chloride, these iron can enter product inevitably, cause the pollution of iron.Therefore, the iron contamination of removing liquor alumini chloridi is to producing highly purified liquor alumini chloridi, and the products such as preparation low iron polymerize aluminum chloride, aluminium chlorohydroxide and low iron crystal aluminum chloride are significant.
But, because there be general being difficult to its removal in iron with highly stable ionic condition in liquor alumini chloridi.Usually adopting aluminium hydroxide or the aluminum oxide processed through deironing in the industrial production is that raw material is produced low iron liquor alumini chloridi.This has limited and has produced the raw material sources of aluminum chloride, and has increased production cost.For because material purity is not enough or be subject to the iron content liquor alumini chloridi of iron pollution, there is not at present suitable method for removing iron.
Summary of the invention
For the deficiencies in the prior art, the purpose of this invention is to provide a kind of method that adopts resins exchange is carried out deep iron removal to liquor alumini chloridi method.
The method of the invention comprises: the liquor alumini chloridi of iron content is passed through resin column, utilize resin that the adsorptive power of iron is carried out deironing, the pH value of wherein said liquor alumini chloridi is 1.0~3.0; Treatment temp is room temperature~90 ℃, and preferable range is 60~80 ℃, the liquor alumini chloridi flow velocity be 1~4 times of resin volume/hour, preferable range be 2~3 times of resin volumes/hour, at last refined crystalline aluminium chloride solution.
As preferred implementation of the present invention, the resin in the resin column is the macroporous type resin cation (R.C.).
Described macroporous type resin cation (R.C.) can be selected D001,732,742,7020H, 7120H, JK008 or SPC-1 etc.
As preferred implementation of the present invention, resin column can adopt the mode of single-column or twin columns series winding.
As preferred implementation of the present invention, when liquor alumini chloridi was processed through resin column, liquor alumini chloridi passed through resin column in the mode of bottom in and top out.
As preferred implementation of the present invention, resin absorption is saturated carries out wash-out and regeneration afterwards to resin, makes resin recover adsorptive power.Elution requirement is: eluting temperature is room temperature~60 ℃, preferable range is 30~50 ℃, eluent employing water or mass concentration are 2~10% hydrochloric acid, preferable range is that mass concentration is 3~5% hydrochloric acid, the eluent consumption is 1~3 times of resin volume, the eluent flow velocity be 1~3 times of resin volume/hour.Temperature is room temperature~60 ℃ during regeneration, and adopting mass concentration is 2~10%, and preferable range is that mass concentration is 3~5% hydrochloric acid, and the hydrochloric acid consumption is 1~2 times of resin volume, the hydrochloric acid flow velocity be 1~3 times of resin volume/hour.
As preferred implementation of the present invention, during wash-out, eluent passes through resin column in the mode of upper entering and lower leaving.
As preferred implementation of the present invention, during regeneration, hydrochloric acid passes through resin column in the mode of upper entering and lower leaving.
After deironing, the concentration of iron can be reduced to below 0.3 mg/litre (in ferric oxide) in the solution.
Usefulness of the present invention is, production technique is simple, and production process is easy to control, the characteristics of constant product quality.Adopt this method, can enlarge the raw material sources of liquor alumini chloridi and subsequent product thereof, reduce production costs.
Embodiment
Below in conjunction with embodiment explanation the present invention, but the present invention is not restricted to this.
Embodiment 1
To contain aluminium 98 grams per liters (in aluminum oxide), iron content 1.5 grams per liters (in ferric oxide), pH value are 1.5, and temperature is 65 ℃ liquor alumini chloridi, be pressed into the resin column of dress D001 (chemical plant, Anhui Province east) resin with noncorrosive pump, carry out deironing with the mode of single-column.During processing the liquor alumini chloridi flow velocity be 2 times of resin volumes/hour.After deironing was processed, the refined crystalline aluminium chloride liquid that obtains contained aluminium 96 grams per liters (in aluminum oxide), and iron content 0.25 mg/litre (in ferric aluminum oxide), pH value are 1.5, and temperature is 55 ℃.
After resin absorption is saturated, make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent adopts water, 40 ℃ of eluting temperatures, flow velocity be 1 times of resin volume/hour, adopt altogether the water of 3 times of resin volumes during wash-out; Adopting mass concentration during regeneration is 5% hydrochloric acid, and temperature is room temperature, the hydrochloric acid flow velocity be 3 times of resin volumes/hour, adopt altogether the hydrochloric acid of 2 times of resin volumes during regeneration.
Embodiment 2
To contain aluminium 80 grams per liters (in aluminum oxide), iron content 1.3 grams per liters (in ferric oxide), the pH value is 1.9, temperature is 75 ℃ liquor alumini chloridi, be pressed into the resin column that fills 732 (Anhui Samsung resin Science and Technology Ltd.) resin with noncorrosive pump, carry out deironing with the mode of twin columns series winding.During processing the liquor alumini chloridi flow velocity be 4 times of resin volumes/hour.After deironing was processed, the refined crystalline aluminium chloride liquid that obtains contained aluminium 78 grams per liters (in aluminum oxide), and iron content 0.20 mg/litre (in ferric oxide), pH value are 1.9, and temperature is 65 ℃.
After resin absorption is saturated, make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent employing mass concentration is 2% hydrochloric acid, 30 ℃ of eluting temperatures, the hydrochloric acid flow velocity be 1 times of resin volume/hour, adopt altogether the hydrochloric acid of 2 times of resin volumes during wash-out; Adopting mass concentration during regeneration is 2% hydrochloric acid, and temperature is room temperature, the hydrochloric acid flow velocity be 2 times of resin volumes/hour, adopt altogether the hydrochloric acid of 1 times of resin volume during regeneration.
Embodiment 3
To contain aluminium 90 grams per liters (in aluminum oxide), iron content 1.4 grams per liters (in ferric oxide), pH value are 1.0, and temperature is 90 ℃ liquor alumini chloridi, be pressed into the resin column that JK008 (chemical plant, Anhui Province east) resin is housed with noncorrosive pump, carry out deironing with the mode of twin columns series winding.During processing the liquor alumini chloridi flow velocity be 3 times of resin volumes/hour.After deironing was processed, the refined crystalline aluminium chloride liquid that obtains contained aluminium 87 grams per liters (in aluminum oxide), and iron content 0.22 mg/litre (in ferric oxide), pH value are 1.0, and temperature is 78 ℃.
After resin absorption is saturated, make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent employing mass concentration is 8% hydrochloric acid, 60 ℃ of eluting temperatures, the hydrochloric acid flow velocity be 3 times of resin volumes/hour, adopt altogether the hydrochloric acid of 2 times of resin volumes during wash-out; Adopting mass concentration during regeneration is 8% hydrochloric acid, and temperature is 50 ℃, the hydrochloric acid flow velocity be 2 times of resin volumes/hour, adopt altogether the hydrochloric acid of 1 times of resin volume during regeneration.

Claims (8)

1. the method for a removing iron from solution of aluminum chloride comprises: by resin column, the pH value of wherein said liquor alumini chloridi is 1.0 ~ 3.0 with the liquor alumini chloridi of iron content; Treatment temp is room temperature ~ 90 ° C; The liquor alumini chloridi flow velocity be 1~4 times of resin volume/hour, at last refined crystalline aluminium chloride solution; Resin is D001,732,742,7020H, 7120H, JK008 or SPC-1 in the described resin column.
2. method according to claim 1 is characterized in that, liquor alumini chloridi is 60 ~ 80 ℃ by the treatment temp of resin column.
3. method according to claim 1 and 2 is characterized in that, the flow velocity of liquor alumini chloridi be 2~3 times of resin volumes/hour.
4. method according to claim 1 is characterized in that, resin column adopts the mode of single-column or twin columns series winding.
5. method according to claim 1, it is characterized in that, resin absorption in the resin column is saturated carries out wash-out and regeneration afterwards to resin, wherein elution requirement is: eluting temperature is room temperature ~ 60 ℃, eluent employing water or mass concentration are 2~10% hydrochloric acid, the eluent consumption is 1~3 times of resin volume, the eluent flow velocity be 1~3 times of resin volume/hour; Temperature is room temperature ~ 60 ℃ during regeneration, and adopting mass concentration is 2 ~ 10% hydrochloric acid, and the hydrochloric acid consumption is 1~2 times of resin volume, the flow velocity of hydrochloric acid be 1~3 times of resin volume/hour.
6. method according to claim 5 is characterized in that, the resin elution temperature is 30 ~ 50 ℃.
7. according to claim 5 or 6 described methods, it is characterized in that, eluent is that water or mass concentration are 3~5% hydrochloric acid.
8. method according to claim 5 is characterized in that, the employing mass concentration is 3~5% hydrochloric acid during regeneration.
CN 201110104081 2010-04-27 2011-04-25 Method for deironing aluminum chloride solution Active CN102249277B (en)

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CN201010161899.7 2010-04-27
CN201010161899A CN101838004A (en) 2010-04-27 2010-04-27 Method for removing iron from solution of aluminum chloride
CN 201110104081 CN102249277B (en) 2010-04-27 2011-04-25 Method for deironing aluminum chloride solution

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Publication number Priority date Publication date Assignee Title
CN103288115B (en) * 2013-05-08 2016-03-16 中国神华能源股份有限公司 The method of impurity metal ion in multistage resin column removing liquor alumini chloridi
CN103435080B (en) * 2013-08-22 2015-12-09 中国神华能源股份有限公司 A kind of method of aluminum chloride slurry extraction deironing
CN106119555B (en) * 2016-06-23 2018-10-12 中国神华能源股份有限公司 A method of extracting scandium from flyash
CN112811468B (en) * 2020-12-25 2023-05-23 四川省绵阳市华意达化工有限公司 Method for improving quality of chromic anhydride

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4652433A (en) * 1986-01-29 1987-03-24 Florida Progress Corporation Method for the recovery of minerals and production of by-products from coal ash
CN86100720A (en) * 1986-02-05 1987-08-26 中国科学院化工冶金研究所 With extracting deironing in the aluminium sulfate solution with tertiary amine

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4652433A (en) * 1986-01-29 1987-03-24 Florida Progress Corporation Method for the recovery of minerals and production of by-products from coal ash
CN86100720A (en) * 1986-02-05 1987-08-26 中国科学院化工冶金研究所 With extracting deironing in the aluminium sulfate solution with tertiary amine

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
蔚龙凤等.用离子交换法生产无铁级硫酸铝.《湿法冶金》.2008,第27卷(第2期),第87页左栏倒数第2行至右栏第1行,第1.1节,第88页第1.2.2节,第89页第2.2.1.1节,图2. *

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