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.