CN103435080B - A kind of method of aluminum chloride slurry extraction deironing - Google Patents
A kind of method of aluminum chloride slurry extraction deironing Download PDFInfo
- Publication number
- CN103435080B CN103435080B CN201310370405.XA CN201310370405A CN103435080B CN 103435080 B CN103435080 B CN 103435080B CN 201310370405 A CN201310370405 A CN 201310370405A CN 103435080 B CN103435080 B CN 103435080B
- Authority
- CN
- China
- Prior art keywords
- organic phase
- extraction
- aluminum chloride
- hydrochloric acid
- acid soln
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 title claims abstract description 138
- 238000000605 extraction Methods 0.000 title claims abstract description 110
- 239000002002 slurry Substances 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000012074 organic phase Substances 0.000 claims abstract description 91
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 88
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000008346 aqueous phase Substances 0.000 claims abstract description 34
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 32
- 238000000926 separation method Methods 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 229910052742 iron Inorganic materials 0.000 claims abstract description 19
- 239000003350 kerosene Substances 0.000 claims abstract description 17
- 239000013078 crystal Substances 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 11
- -1 trioctylphosphine tertiary amine Chemical class 0.000 claims description 11
- SJWFXCIHNDVPSH-UHFFFAOYSA-N octan-2-ol Chemical compound CCCCCCC(C)O SJWFXCIHNDVPSH-UHFFFAOYSA-N 0.000 claims description 8
- LJKDOMVGKKPJBH-UHFFFAOYSA-N 2-ethylhexyl dihydrogen phosphate Chemical class CCCCC(CC)COP(O)(O)=O LJKDOMVGKKPJBH-UHFFFAOYSA-N 0.000 claims description 7
- 230000001186 cumulative effect Effects 0.000 claims description 7
- DNVCVNWQDMXRNF-UHFFFAOYSA-N n-octan-2-ylacetamide Chemical compound CCCCCCC(C)NC(C)=O DNVCVNWQDMXRNF-UHFFFAOYSA-N 0.000 claims description 7
- 238000000746 purification Methods 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims 1
- 238000003756 stirring Methods 0.000 description 13
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000004064 recycling Methods 0.000 description 7
- 239000010865 sewage Substances 0.000 description 7
- 238000013517 stratification Methods 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 6
- 229910001570 bauxite Inorganic materials 0.000 description 4
- 239000010881 fly ash Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229940024546 aluminum hydroxide gel Drugs 0.000 description 1
- SMYKVLBUSSNXMV-UHFFFAOYSA-K aluminum;trihydroxide;hydrate Chemical compound O.[OH-].[OH-].[OH-].[Al+3] SMYKVLBUSSNXMV-UHFFFAOYSA-K 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention provides the method for a kind of aluminum chloride slurry extraction deironing, comprise the steps: that solid content is that the pH value of the aluminum chloride slurry of the iron content of 30wt% ~ 60wt% is adjusted to 1 ~ 3 with hydrochloric acid soln by (1); (2) preparation comprises the extracted organic phase of extraction agent and sulfonated kerosene, and the volume of described extraction agent accounts for the 30vol%-60vol% of this extracted organic phase volume; (3) mixed to extract with extracted organic phase by slurries, be separated organic phase and aqueous phase after reaching extraction equilibrium, described aqueous phase is the aluminum chloride slurry after extraction; (4) aluminum chloride slurry after extraction is carried out solid-liquid separation, the liquor alumini chloridi after obtaining crystal aluminum chloride product and being separated; (5) organic phase is mixed with hydrochloric acid soln, carry out stripping to reclaim organic phase.The usage quantity of organic phase when method of the present invention can reduce extraction, the volume of the extraction equipment is simultaneously minimized.
Description
Technical field
The present invention relates to a kind of purification process of aluminum chloride, the method for particularly a kind of aluminum chloride slurry extraction deironing.
Background technology
China's bauxite resource is very abundant, extracts a large amount of aluminium every year from bauxite, coal gangue, flyash.In the leaching process of aluminium, hydrochloric acid acid pasting can be adopted to produce liquor alumini chloridi, solution is concentrated further obtains crystal aluminum chloride.Crystal aluminum chloride is a kind of important Chemicals, commonly uses and does coagulating agent, water sanitising agent, also can be used for aluminum hydroxide gel and produces and metallurgical-grade aluminum oxide production.But the crystal aluminum chloride that bauxite or the stripping of flyash hydrochloric acid, crystallization obtain contains iron(ic) chloride composition, and the existence of ferro element can affect the quality of crystal aluminum chloride product.
In industrial production, the main removing iron from solution of aluminum chloride method adopted comprises: chemical precipitation method, resin adsorption method and solution extraction etc.Solvent extration deironing make use of the difference of iron ion solubleness or partition ratio in two kinds of immiscible solvents, and iron ion is moved on to organic solvent from Transfer in Aqueous Solution.At present, generally can produce the liquor alumini chloridi of 100-250g/L with salt acid soak bauxite and flyash, by conventional extraction process, the organic reagent volume that extraction liquor alumini chloridi is used is suitable with liquor alumini chloridi, 1m
3liquor alumini chloridi roughly needs 1m
3organic solvent, and the extraction tank needing volume to adapt.Because liquor alumini chloridi amount in Industrial processes is large, therefore need large-scale extraction equipment, and need the extraction agent of at substantial.
At present, not yet occur that a kind of extraction agent usage quantity is less, do not need the method for the aluminum chloride slurry extraction deironing of large-scale extraction equipment simultaneously.
Summary of the invention
In order to overcome the defect of prior art, present inventor conducts in-depth research.
The object of the present invention is to provide a kind of aluminum chloride slurry to extract the method for deironing, the extraction agent usage quantity of the method is less, do not need large-scale extraction equipment simultaneously.
The invention provides the method for a kind of aluminum chloride slurry extraction deironing, comprise the steps:
(1) be that the pH value of aluminum chloride slurry of iron content of 30wt% ~ 60wt% is adjusted to 1 ~ 3 by solid content with hydrochloric acid soln;
(2) preparation comprises the extracted organic phase of extraction agent and sulfonated kerosene; the volume of described extraction agent accounts for the 30vol%-60vol% of this extracted organic phase volume; wherein said extraction agent is selected from two (2-ethylhexyl phosphoric acids), tbp, N; N '-two (1-methylheptyl) ethanamide, trioctylphosphine tertiary amine, one or more in sec-octyl alcohol;
(3) extracted organic phase that slurries step (1) obtained and step (2) obtain mixes to extract, and is separated organic phase and aqueous phase after reaching extraction equilibrium, and described aqueous phase is the aluminum chloride slurry after extraction;
(4) aluminum chloride slurry after the extraction of step (3) is carried out solid-liquid separation, the liquor alumini chloridi after obtaining crystal aluminum chloride product and being separated;
(5) organic phase of step (3) is mixed with hydrochloric acid soln, carry out stripping to reclaim organic phase.
In the present invention, step (1) is the pH value of the aluminum chloride slurry regulating iron content with hydrochloric acid soln.The concentration of this hydrochloric acid soln does not limit especially.Preferably, the concentration of this hydrochloric acid soln can be 1-5wt%, is more preferably 2-3wt%.The pH value of the aluminum chloride slurry of the iron content after adjustment can be 1 ~ 3, is preferably 2-2.5, is more preferably 2.1-2.3.The solid content of the aluminum chloride slurry of iron content can be 30wt% ~ 60wt%, is preferably 35wt% ~ 55wt%, is more preferably 40wt% ~ 50wt%.
In the present invention, step (2) is the step of preparation extracted organic phase.The method of preparation is not particularly limited, such as, each component can be mixed.This extracted organic phase can comprise extraction agent and sulfonated kerosene.This extracted organic phase can also comprise other suitable thinners, and other suitable thinners are known in the art those, repeat no more here.Preferably, this extracted organic phase is made up of extraction agent and sulfonated kerosene.
In the present invention, the volume of described extraction agent accounts for the 30vol%-60vol% of this extracted organic phase volume, is preferably 35vol%-55vol%, is more preferably 40vol%-50vol%.
In the present invention, described extraction agent is selected from two (2-ethylhexyl phosphoric acids), tbp, N, N '-two (1-methylheptyl) ethanamide, trioctylphosphine tertiary amine, one or more in sec-octyl alcohol.Preferably, extraction agent of the present invention is selected from two (2-ethylhexyl phosphoric acids), tbp, N, N '-two (1-methylheptyl) ethanamide, trioctylphosphine tertiary amine, one or both in sec-octyl alcohol.More preferably, extraction agent of the present invention is selected from two (2-ethylhexyl phosphoric acids), tbp, N, N '-two (1-methylheptyl) ethanamide, trioctylphosphine tertiary amine, the one in sec-octyl alcohol.Again preferably, extraction agent of the present invention is the mixture of tbp and sec-octyl alcohol.
In the present invention, step (3) is extraction step, and wherein, described extracted organic phase can account for the 30vol% ~ 70vol% of the cumulative volume of slurries and extracted organic phase, is preferably 40vol% ~ 65vol%, is more preferably 50vol% ~ 60vol%.
In the present invention, in step (3), extraction temperature can be 20 ~ 80 DEG C, and extraction time can be 0.1 ~ 2 hour.Preferably, extraction temperature can be 30 ~ 70 DEG C, and extraction time can be 0.2 ~ 1.5 hour; More preferably, extraction temperature can be 35 ~ 50 DEG C, and extraction time can be 0.3 ~ 1 hour.
In step of the present invention (3), above-mentioned extracted organic phase and slurries are mixed in extraction tank, leave standstill after, organic phase and aqueous phase are divided into two-layer up and down.The overflow device organic phase on upper strata arranged in extraction tank is extracted out, residual lower floor aqueous phase, and it is the aluminum chloride slurry after extraction.In aluminum chloride slurry after extraction, iron-holder reduces greatly, preferably at 0.0025-0.05g/L.
In the present invention, step (4) is solid-liquid separation step.Liquor alumini chloridi after obtaining crystal aluminum chloride product by solid-liquid separation and be separated.The method be separated is not particularly limited.But as preferably, whizzer separation can be adopted, revolving-leaf type filter is separated or band filter is separated.
According to the present invention one preferred embodiment, step (4) adopts whizzer to carry out solid-liquid separation.The rotating speed of whizzer can for 500-20000rpm(namely rev/min, lower with), be preferably 1000-10000rpm.
According to the present invention another preferred embodiment, step (4) adopts revolving-leaf type filter or band filter to carry out solid-liquid separation.Vacuum tightness when adopting revolving-leaf type filter or band filter to carry out solid-liquid separation can be 0.035MPa ~ 0.08MPa, is preferably 0.04MPa ~ 0.07MPa, is more preferably 0.05MPa ~ 0.06MPa.Rotating speed when adopting revolving-leaf type filter to carry out solid-liquid separation can be 0.2-8rpm, is preferably 0.5-1rpm.
By step of the present invention (4), the liquor alumini chloridi after obtaining crystal aluminum chloride product and being separated.Liquor alumini chloridi after being separated is returned vapo(u)rization system.The iron-holder of crystal aluminum chloride product is significantly reduced.
In the present invention, step (5) is strip stage.The organic phase of step (3) is mixed with hydrochloric acid soln, carries out stripping to reclaim organic phase.In step (5), the concentration of hydrochloric acid soln can be 1 ~ 8mol/L, is preferably 1.5 ~ 6mol/L, is more preferably 2 ~ 5mol/L.The volume of hydrochloric acid soln accounts for the 40vol% ~ 60vol% of the cumulative volume of hydrochloric acid soln and organic phase, and preferably, the volume of hydrochloric acid soln accounts for the 50vol% ~ 52vol% of the cumulative volume of hydrochloric acid soln and organic phase.More preferably, the volume of hydrochloric acid soln accounts for the 50vol% ~ 51vol% of the cumulative volume of hydrochloric acid soln and organic phase.
In the present invention, step (5) can be carried out in separating funnel.The organic phase of step (3) is mixed with hydrochloric acid soln, then stirs 0.5-5 hour, be preferably 1-3 hour.After stratification, be separated organic phase and aqueous phase.Be separated the organic phase obtained and return the extraction agent recycling of extracting system as the aluminum chloride slurry after extraction; Aqueous phase after separation enters Sewage treatment systems.
Adopt method of the present invention to carry out deironing process to the aluminum chloride slurry of iron content, decrease the use of extraction agent, reduce the volume of required extraction equipment simultaneously.
Embodiment
Further describe the present invention below in conjunction with embodiment, but the present invention is not therefore subject to any restriction.In the present invention, vol% represents volumn concentration, and wt% represents weight percentage.
Embodiment 1
Get the aluminum chloride slurry that solid content is the iron content of 30wt%, with the hydrochloric acid soln of 4wt%, the pH value of these slurries is adjusted to 1, for subsequent use.
Preparation extracted organic phase, for subsequent use.The formula of this extracted organic phase is: 30vol% trioctylphosphine tertiary amine and 70vol% sulfonated kerosene.Wherein, be extraction agent with trioctylphosphine tertiary amine (N235, Luoyang Ao Da Chemical Co., Ltd. produces), with sulfonated kerosene (production of Bao Run Chemical Co., Ltd.) for thinner.
Above-mentioned extracted organic phase and slurries are mixed in extraction tank by the volume shown in table 1, controlling extraction temperature is 20 DEG C, stirs 0.1 hour in extraction tank, leaves standstill 0.1 hour.Until organic phase and aqueous phase be divided into two-layer up and down after, the overflow device organic phase on upper strata arranged in extraction tank is extracted out, residual lower floor aqueous phase, and it be the aluminum chloride slurry after extracting.
Adopt whizzer that the aluminum chloride slurry after above-mentioned extraction is carried out solid-liquid separation, centrifuge speed is 1000 revs/min, the liquor alumini chloridi after obtaining crystal aluminum chloride product and being separated.Liquor alumini chloridi after being separated is returned vapo(u)rization system.
In separating funnel, adopt the hydrochloric acid soln of 1mol/L to strip to the organic phase of being extracted out by overflow device, this hydrochloric acid soln volume accounts for total mixed solution (i.e. mixed solution of organic phase and hydrochloric acid soln, the 40vol% of volume down together), stir 0.5 hour, after stratification, be separated organic phase and aqueous phase.Be separated the organic phase obtained and return the extraction agent recycling of extracting system as the aluminum chloride slurry after extraction; Aqueous phase after separation enters Sewage treatment systems.
Concrete technology parameter and product property are see table 1.
Embodiment 2
Get the aluminum chloride slurry that solid content is the iron content of 40wt%, with the hydrochloric acid soln of 4wt%, the pH value of these slurries is adjusted to 2.
Preparation extracted organic phase, for subsequent use.The formula of this extracted organic phase is: two (the 2-ethylhexyl phosphoric acids) of 40vol% and the sulfonated kerosene of 60vol%.Wherein, be extraction agent with two (2-ethylhexyl phosphoric acids) (P204, Shanggao County, Jiangxi Yong Sheng Chemical Co., Ltd. produces), with sulfonated kerosene (production of Bao Run Chemical Co., Ltd.) for thinner.
Above-mentioned extracted organic phase and slurries are mixed in extraction tank by the volume described in table 1, controlling extraction temperature is 30 DEG C, stirs 1 hour in extraction tank, leaves standstill 0.1 hour.Until organic phase and aqueous phase be divided into two-layer up and down after, the overflow device organic phase on upper strata arranged in extraction tank is extracted out, residual lower floor aqueous phase, and it be the aluminum chloride slurry after extracting.
Adopt revolving-leaf type filter that the aluminum chloride slurry after above-mentioned extraction is carried out solid-liquid separation, revolving-leaf type filter rotating speed is 0.5 rev/min, and vacuum tightness is 0.035MPa, the liquor alumini chloridi after obtaining crystal aluminum chloride product and being separated.Liquor alumini chloridi after separation returns vapo(u)rization system.
In separating funnel, adopt the hydrochloric acid soln of 3mol/L to strip to the organic phase of being extracted out by overflow device, this hydrochloric acid soln volume accounts for the 40vol% of total mixeding liquid volume, stirs 0.5 hour, after stratification, is separated organic phase and aqueous phase.Be separated the organic phase obtained and return the extraction agent recycling of extracting system as the aluminum chloride slurry after extraction; Aqueous phase enters Sewage treatment systems.
Concrete technology parameter and product property are see table 1.
Embodiment 3
Get the aluminum chloride slurry that solid content is the iron content of 50wt%, with the hydrochloric acid soln of 4wt%, the pH value of these slurries is adjusted to 3.
Preparation extracted organic phase, for subsequent use.The formula of this extracted organic phase is: 50vol% tbp and 50vol% sulfonated kerosene.Wherein, be extraction agent with tbp (TBP, Shanggao County, Jiangxi Yong Sheng Chemical Co., Ltd. produces), with sulfonated kerosene (production of Bao Run Chemical Co., Ltd.) for thinner.
Above-mentioned extracted organic phase and slurries are mixed in extraction tank by the volume shown in table 1, controlling extraction temperature is 40 DEG C, stirs 1.5 hours in extraction tank, leaves standstill 0.1 hour.Until organic phase and aqueous phase be divided into two-layer up and down after, the overflow device organic phase on upper strata arranged in extraction tank is extracted out, residual lower floor aqueous phase, and it be the aluminum chloride slurry after extracting.
Adopt revolving-leaf type filter the aluminum chloride slurry after described extraction to be carried out solid-liquid separation, revolving-leaf type filter rotating speed 1.0 revs/min, vacuum tightness is 0.045MPa, the liquor alumini chloridi after obtaining crystal aluminum chloride product and being separated.Liquor alumini chloridi after separation returns vapo(u)rization system.
In separating funnel, adopt 5mol/L hydrochloric acid soln to strip to the organic phase of being extracted out by overflow device, this hydrochloric acid soln accounts for the 50vol% of total mixeding liquid volume, stirs 1.0 hours, after stratification, is separated organic phase and aqueous phase.Be separated the organic phase obtained and return the extraction agent recycling of extracting system as the aluminum chloride slurry after extraction; Aqueous phase enters Sewage treatment systems.
Concrete technology parameter and product property are see table 1.
Embodiment 4
Get the aluminum chloride slurry that solid content is the iron content of 60wt%, with the hydrochloric acid soln of 4wt%, the pH value of these slurries is adjusted to 2.
Preparation extracted organic phase, for subsequent use.The formula of this extracted organic phase is: the N of 60vol%, N '-two sulfonated kerosene of (1-methylheptyl) ethanamide and 40vol%.Wherein, with N, N, '-two (1-methylheptyl) ethanamide (N1923, Run Da Chemical Co., Ltd. of Liyang City produces) is extraction agent, with sulfonated kerosene (production of Bao Run Chemical Co., Ltd.) for thinner.
Above-mentioned extracted organic phase and slurries are mixed in extraction tank by the volume shown in table 1, controlling extraction temperature is 80 DEG C, stirs 2 hours in extraction tank, leaves standstill 0.1 hour.Until organic phase and aqueous phase be divided into two-layer up and down after, the overflow device organic phase on upper strata arranged in extraction tank is extracted out, residual lower floor aqueous phase, and it be the aluminum chloride slurry after extracting.
Adopt band filter that the aluminum chloride slurry after described extraction is carried out solid-liquid separation, band filter vacuum tightness is 0.06MPa, the liquor alumini chloridi after obtaining crystal aluminum chloride product and being separated.Liquor alumini chloridi after separation returns vapo(u)rization system.
In separating funnel, adopt 8mol/L hydrochloric acid soln to strip to the organic phase of being extracted out by overflow device, this hydrochloric acid soln accounts for the 50vol% of total mixeding liquid volume, stirs 1.0 hours, after stratification, is separated organic phase and aqueous phase.Be separated the organic phase obtained and return the extraction agent recycling of extracting system as the aluminum chloride slurry after extraction; Aqueous phase enters Sewage treatment systems.
Concrete technology parameter and product property are see table 1.
Embodiment 5
Get the aluminum chloride slurry of the iron content of solid content 60wt%, with 4% hydrochloric acid soln, the pH value of these slurries is adjusted to 2.
Preparation extracted organic phase, for subsequent use.The formula of this extracted organic phase is: 50vol% sec-octyl alcohol and 50vol% sulfonated kerosene.Wherein, with sec-octyl alcohol (production of Shanghai De Mao Chemical Co., Ltd.) for extraction agent, with sulfonated kerosene (production of Bao Run Chemical Co., Ltd.) for thinner.
Above-mentioned extracted organic phase and slurries are mixed in extraction tank by the volume shown in table 1, controlling extraction temperature is 50 DEG C, stirs 2 hours in extraction tank, leaves standstill 0.1 hour.Until organic phase and aqueous phase be divided into two-layer up and down after, the overflow device organic phase on upper strata arranged in extraction tank is extracted out, residual lower floor aqueous phase, and it be the aluminum chloride slurry after extracting.
Adopt band filter that the aluminum chloride slurry after described extraction is carried out solid-liquid separation, band filter vacuum tightness is 0.08MPa, the liquor alumini chloridi after obtaining crystal aluminum chloride product and being separated.Liquor alumini chloridi after separation returns vapo(u)rization system.
In separating funnel, adopt 6mol/L hydrochloric acid soln to strip to the organic phase of being extracted out by overflow device, this hydrochloric acid soln accounts for the 60vol% of total mixeding liquid volume, stirs 1.0 hours, after stratification, is separated organic phase and aqueous phase.Be separated the organic phase obtained and return the extraction agent recycling of extracting system as the aluminum chloride slurry after extraction; Aqueous phase enters Sewage treatment systems.
Concrete technology parameter and product property are see table 1.
Embodiment 6
Get the aluminum chloride slurry of the iron content of solid content 60wt%, with the hydrochloric acid soln of 4wt%, the pH value of these slurries is adjusted to 2.
Preparation extracted organic phase, for subsequent use.The formula of this extracted organic phase is: 30vol% trioctylphosphine tertiary amine, 20vol% tbp and 50vol% sulfonated kerosene.Wherein, be mixed extractant with trioctylphosphine tertiary amine (N235, Luoyang Ao Da Chemical Co., Ltd. produces) and tbp (TBP, Shanggao County, Jiangxi Yong Sheng Chemical Co., Ltd. produces), with sulfonated kerosene (production of Bao Run Chemical Co., Ltd.) for thinner.
Above-mentioned extracted organic phase and slurries are mixed in extraction tank by the volume shown in table 1, controlling extraction temperature is 30 DEG C, stirs 2 hours in extraction tank, leaves standstill 0.1 hour.Until organic phase and aqueous phase be divided into two-layer up and down after, the overflow device organic phase on upper strata arranged in extraction tank is extracted out, residual lower floor aqueous phase, and it be the aluminum chloride slurry after extracting.
Adopt band filter that the aluminum chloride slurry after described extraction is carried out solid-liquid separation, band filter vacuum tightness is 0.04MPa, the liquor alumini chloridi after obtaining crystal aluminum chloride product and being separated.Liquor alumini chloridi after separation returns vapo(u)rization system.
In separating funnel, adopt 7mol/L hydrochloric acid soln to strip to the organic phase of being extracted out by overflow device, this hydrochloric acid soln accounts for the 60vol% of total mixeding liquid volume, stirs 1.0 hours, after stratification, is separated organic phase and aqueous phase.Be separated the organic phase obtained and return the extraction agent recycling of extracting system as the aluminum chloride slurry after extraction; Aqueous phase enters Sewage treatment systems.
Concrete technology parameter and product property are see table 1.
Comparative example 1
Aluminum chloride slurry except the iron content by solid content being 40wt% replaces with the liquor alumini chloridi that concentration is 150g/L, and other conditions are identical with embodiment 1.
Table 1, concrete technology parameter and product property
As shown in Table 1, compared with comparative example 1, adopt method of the present invention to carry out extraction deironing to the aluminum chloride slurry of iron content, the volume of required extracted organic phase is smaller, and thus the volume of extraction tank also can correspondingly reduce.As can be seen here, the present invention has the advantage of the few and extraction equipment miniaturization of organic reagent consumption.
Above-described embodiment is used for illustrative purposes only; and be not limitation of the present invention; the those of ordinary skill of relevant technical field; without departing from the spirit and scope of the present invention; can also make a variety of changes and modification; therefore all equivalent technical schemes also should belong to category of the present invention, and scope of patent protection of the present invention should be limited by each claim.
Claims (8)
1. a purification process for aluminum chloride, carries out extraction deironing to aluminum chloride slurry, comprises the steps:
(1) be that the pH value of aluminum chloride slurry of iron content of 35wt% ~ 55wt% is adjusted to 2 ~ 2.5 by solid content with hydrochloric acid soln;
(2) preparation comprises the extracted organic phase of extraction agent and sulfonated kerosene, the volume of described extraction agent accounts for the 30vol%-60vol% of this extracted organic phase volume, wherein said extraction agent be selected from two (2-ethylhexyl phosphoric acids), tbp, N, N '-two (1-methylheptyl) ethanamide, trioctylphosphine tertiary amine, sec-octyl alcohol one or more;
(3) extracted organic phase that slurries step (1) obtained and step (2) obtain mixes to extract, and is separated organic phase and aqueous phase after reaching extraction equilibrium, and described aqueous phase is the aluminum chloride slurry after extraction;
(4) aluminum chloride slurry after the extraction of step (3) is carried out solid-liquid separation, the liquor alumini chloridi after obtaining crystal aluminum chloride product and being separated;
(5) organic phase of step (3) is mixed with hydrochloric acid soln, carry out stripping to reclaim organic phase;
Wherein, in step (3), described extracted organic phase accounts for the 30vol% ~ 70vol% of the cumulative volume of slurries and extracted organic phase.
2. method according to claim 1, is characterized in that, in step (3), extraction temperature is 20 ~ 80 DEG C, and extraction time is 0.1 ~ 2 hour.
3. method according to claim 1, is characterized in that, in step (5), the concentration of hydrochloric acid soln is 1 ~ 8mol/L.
4. method according to claim 3, is characterized in that, in step (5), the volume of hydrochloric acid soln accounts for the 40vol% ~ 60vol% of the cumulative volume of hydrochloric acid soln and organic phase.
5. method according to claim 4, is characterized in that, in step (5), the volume of hydrochloric acid soln accounts for the 50vol% ~ 52vol% of the cumulative volume of hydrochloric acid soln and organic phase.
6. method according to claim 1, is characterized in that, in step (4), adopts the mode of centrifugation to carry out solid-liquid separation.
7. method according to claim 1, is characterized in that, in step (4), adopts revolving-leaf type filter or band filter to carry out solid-liquid separation.
8. method according to claim 7, is characterized in that, vacuum tightness when adopting revolving-leaf type filter or band filter to carry out solid-liquid separation is 0.035MPa ~ 0.08MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310370405.XA CN103435080B (en) | 2013-08-22 | 2013-08-22 | A kind of method of aluminum chloride slurry extraction deironing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310370405.XA CN103435080B (en) | 2013-08-22 | 2013-08-22 | A kind of method of aluminum chloride slurry extraction deironing |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103435080A CN103435080A (en) | 2013-12-11 |
| CN103435080B true CN103435080B (en) | 2015-12-09 |
Family
ID=49688833
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310370405.XA Active CN103435080B (en) | 2013-08-22 | 2013-08-22 | A kind of method of aluminum chloride slurry extraction deironing |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103435080B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104451145B (en) * | 2014-11-25 | 2017-08-11 | 中国科学院青海盐湖研究所 | Extraction is except the method for iron in a kind of mixed solution from chloride |
| CN104946889B (en) * | 2015-06-11 | 2017-10-27 | 广州绿华环保科技有限公司 | A kind of method of extract and separate iron and aluminium from hydrochloric acid medium |
| CN106745142B (en) * | 2017-01-19 | 2018-01-26 | 济南大学 | A kind of extracting process for preparing high-purity aluminium chloride |
| CN111439821B (en) * | 2019-01-17 | 2022-11-01 | 有研稀土新材料股份有限公司 | Method for recovering organic matters in organic matter-containing aqueous solution |
| CN110844963A (en) * | 2019-11-21 | 2020-02-28 | 神华准能资源综合开发有限公司 | Method for separating and recovering aluminum-containing high-iron-salt-acid wastewater |
| CN112390320A (en) * | 2020-10-30 | 2021-02-23 | 神华准能资源综合开发有限公司 | Extraction agent composition and resource utilization method of iron-containing wastewater |
| CN112481497A (en) * | 2020-10-30 | 2021-03-12 | 神华准能资源综合开发有限公司 | Method for removing heavy metal from aluminum-containing hydrochloric acid wastewater |
| CN114702054A (en) * | 2022-04-13 | 2022-07-05 | 衡阳市建衡实业有限公司 | Production process of high-purity polyaluminum chloride |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101509072A (en) * | 2009-02-18 | 2009-08-19 | 中南大学 | Method for extracting valuable metals from laterite nickel mine with hydrochloric acid full-closed circulation method |
| CN101838004A (en) * | 2010-04-27 | 2010-09-22 | 中国神华能源股份有限公司 | Method for removing iron from solution of aluminum chloride |
| WO2013037054A1 (en) * | 2011-09-16 | 2013-03-21 | Orbite Aluminae Inc. | Processes for preparing alumina and various other products |
-
2013
- 2013-08-22 CN CN201310370405.XA patent/CN103435080B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101509072A (en) * | 2009-02-18 | 2009-08-19 | 中南大学 | Method for extracting valuable metals from laterite nickel mine with hydrochloric acid full-closed circulation method |
| CN101838004A (en) * | 2010-04-27 | 2010-09-22 | 中国神华能源股份有限公司 | Method for removing iron from solution of aluminum chloride |
| WO2013037054A1 (en) * | 2011-09-16 | 2013-03-21 | Orbite Aluminae Inc. | Processes for preparing alumina and various other products |
Non-Patent Citations (1)
| Title |
|---|
| 酸法处理铝土矿的浸出液中铁铝分离研究;曲海翠;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;20111231(第S1期);第16-17,22-28页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103435080A (en) | 2013-12-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103435080B (en) | A kind of method of aluminum chloride slurry extraction deironing | |
| CN103787375B (en) | A kind of method extracting rubidium salt and cesium salt | |
| CN103361486B (en) | Method for extracting high purity scandium oxide and titanium from waste acid solution containing scandium and titanium | |
| CN101698488B (en) | Method for preparing lithium carbonate by using salt lake brine with high magnesium-to-lithium ratio | |
| CN103572071B (en) | A kind of method of refining lithium from salt lake brine with high magnesium-lithium ratio | |
| CN106319218A (en) | Method for recovering rare earth, aluminum and silicon from rare earth-containing aluminum and silicon wastes | |
| CN104928475B (en) | A kind of recovery method of the aluminium scrap silicon containing rare earth | |
| CN104745823B (en) | Method for recycling lithium from waste lithium ion battery | |
| CN105692659A (en) | Method for extracting lithium from fly ash | |
| CN106111051B (en) | Iron, aluminum are extracted in a kind of red mud for the method and application of adsorbent | |
| CN103991898B (en) | A kind of catalytic coal gasifaction lime-ash utilize method | |
| CN104928504B (en) | A kind of recovery method of aluminium scrap silicon middle rare earth | |
| CN102127642A (en) | Method for enriching rare-earth elements from red mud | |
| WO2017121343A1 (en) | Process for recovering lithium from industrial wastewater | |
| CN102268552A (en) | Method for preparing scandium oxide by using alumina red mud | |
| CN109811149A (en) | A kind of back extraction and regeneration method of extracting and separating rear earth ionic liquid | |
| CN103436719B (en) | From mixing the lutecium oxide and recovery method that reclaim Cerium aluminate lutetium scintillation crystal waste | |
| CN104789800B (en) | The method that rubidium is extracted from salt lake bittern | |
| CN109680169B (en) | P204 polyaniline-doped solid phase extractant and method for extracting light rare earth by using same | |
| CN110106356B (en) | Method for separating lithium from salt lake brine by using powder type titanium ion exchanger | |
| CN106145443A (en) | A kind of processing method of Rare Earth Production waste water | |
| CN103332699B (en) | A kind of sodium silicate deferrization method | |
| CN105112693A (en) | Method for pressure leaching of rhenium in rhenium-rich slag | |
| CN114807601A (en) | Method for adsorbing rare earth element lanthanum by using phosphoric acid modified kaolin | |
| CN104232897A (en) | Lithium ion extraction system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |