CN102249277A - Method for deironing aluminum chloride solution - Google Patents
Method for deironing aluminum chloride solution Download PDFInfo
- Publication number
- CN102249277A CN102249277A CN 201110104081 CN201110104081A CN102249277A CN 102249277 A CN102249277 A CN 102249277A CN 201110104081 CN201110104081 CN 201110104081 CN 201110104081 A CN201110104081 A CN 201110104081A CN 102249277 A CN102249277 A CN 102249277A
- Authority
- CN
- China
- Prior art keywords
- resin
- hydrochloric acid
- aluminum chloride
- liquor alumini
- alumini chloridi
- 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.)
- Granted
Links
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000011347 resin Substances 0.000 claims abstract description 70
- 229920005989 resin Polymers 0.000 claims abstract description 70
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 51
- 229910052742 iron Inorganic materials 0.000 claims abstract description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 54
- 230000008929 regeneration Effects 0.000 claims description 15
- 238000011069 regeneration method Methods 0.000 claims description 15
- 239000003480 eluent Substances 0.000 claims description 11
- 238000010828 elution Methods 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 229920006395 saturated elastomer Polymers 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 150000001768 cations Chemical class 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 239000004411 aluminium Substances 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 6
- 230000000274 adsorptive effect Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- -1 aluminium chlorohydroxide Chemical compound 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000009972 noncorrosive effect Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000007812 deficiency Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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
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 degree of depth deironing to liquor alumini chloridi method.
Background technology
Liquor alumini chloridi is the important liquid starting material of 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 ionic form.In the process of 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 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 handled 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 subjected to the iron content liquor alumini chloridi of iron pollution, there is not suitable method for removing iron at present.
Summary of the invention
At 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 degree of depth deironing to liquor alumini chloridi method.
The method of the invention comprises: by resin column, utilize resin that the adsorptive power of iron is carried out deironing ferruginous liquor alumini chloridi, 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. for use.
As preferred implementation of the present invention, resin column can adopt the mode of single-column or twin columns polyphone.
As preferred implementation of the present invention, when liquor alumini chloridi was handled through resin column, the mode that goes out on advancing below the liquor alumini chloridi was passed through resin column.
As preferred implementation of the present invention, wash-out and regeneration are carried out to resin in the saturated back of resin absorption, make 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 enterprising mode that goes out down.
As preferred implementation of the present invention, during regeneration, hydrochloric acid passes through resin column in the enterprising mode that goes out down.
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 that 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), the pH value is 1.5, temperature is 65 ℃ a liquor alumini chloridi, is pressed into the resin column of adorning D001 (Wan Dong chemical plant, Anhui) resin with noncorrosive pump, carries 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 handled, 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 the water of 3 times of resin volumes during wash-out altogether; Adopting mass concentration during regeneration is 5% hydrochloric acid, and temperature is a room temperature, the hydrochloric acid flow velocity be 3 times of resin volumes/hour, adopt the hydrochloric acid of 2 times of resin volumes during regeneration altogether.
Embodiment 2
To contain aluminium 80 grams per liters (in aluminum oxide), iron content 1.3 grams per liters (in ferric oxide), pH value are 1.9, and temperature is 75 ℃ a liquor alumini chloridi, be pressed into the resin column of adorning 732 (Anhui Samsung resin Science and Technology Ltd.) resin with noncorrosive pump, carry out deironing with the mode of twin columns polyphone.During processing the liquor alumini chloridi flow velocity be 4 times of resin volumes/hour.After deironing was handled, 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 the hydrochloric acid of 2 times of resin volumes during wash-out altogether; Adopting mass concentration during regeneration is 2% hydrochloric acid, and temperature is a room temperature, the hydrochloric acid flow velocity be 2 times of resin volumes/hour, adopt the hydrochloric acid of 1 times of resin volume during regeneration altogether.
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 ℃ a liquor alumini chloridi, be pressed into the resin column that JK008 (Wan Dong chemical plant, Anhui) resin is housed with noncorrosive pump, carry out deironing with the mode of twin columns polyphone.During processing the liquor alumini chloridi flow velocity be 3 times of resin volumes/hour.After deironing was handled, 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 the hydrochloric acid of 2 times of resin volumes during wash-out altogether; 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 the hydrochloric acid of 1 times of resin volume during regeneration altogether.
Claims (10)
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 ferruginous liquor alumini chloridi; Treatment temp is room temperature～90 ℃; The liquor alumini chloridi flow velocity be 1～4 times of resin volume/hour, at last refined crystalline aluminium chloride solution.
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 polyphone.
5. method according to claim 1 is characterized in that, resin is the macroporous type resin cation (R.C.) in the resin column.
6. method according to claim 5 is characterized in that, resin is D001,732,742,7020H, 7120H, JK008 or SPC-1.
7. method according to claim 1, it is characterized in that, wash-out and regeneration are carried out to resin in the saturated back of resin absorption in the resin column, 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.
8. method according to claim 7 is characterized in that, the resin elution temperature is 30～50 ℃.
9. according to claim 7 or 8 described methods, it is characterized in that eluent is that water or mass concentration are 3～5% hydrochloric acid.
10. method according to claim 7 is characterized in that, the employing mass concentration is 3～5% hydrochloric acid during regeneration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110104081 CN102249277B (en) | 2010-04-27 | 2011-04-25 | Method for deironing aluminum chloride solution |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102249277A true CN102249277A (en) | 2011-11-23 |
| CN102249277B CN102249277B (en) | 2013-04-17 |
Family
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Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010161899A Pending CN101838004A (en) | 2010-04-27 | 2010-04-27 | Method for removing iron from solution of aluminum chloride |
| CN 201110104081 Active CN102249277B (en) | 2010-04-27 | 2011-04-25 | Method for deironing aluminum chloride solution |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010161899A Pending CN101838004A (en) | 2010-04-27 | 2010-04-27 | Method for removing iron from solution of aluminum chloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN101838004A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106119555A (en) * | 2016-06-23 | 2016-11-16 | 中国神华能源股份有限公司 | A kind of method extracting scandium from flyash |
| CN112811468A (en) * | 2020-12-25 | 2021-05-18 | 四川省绵阳市华意达化工有限公司 | Method for improving quality of chromic anhydride |
Families Citing this family (2)
| 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 |
Citations (2)
| 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 |
-
2010
- 2010-04-27 CN CN201010161899A patent/CN101838004A/en active Pending
-
2011
- 2011-04-25 CN CN 201110104081 patent/CN102249277B/en active Active
Patent Citations (2)
| 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)
| Title |
|---|
| 《湿法冶金》 20080630 蔚龙凤等 用离子交换法生产无铁级硫酸铝 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 1-10 第27卷, 第2期 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106119555A (en) * | 2016-06-23 | 2016-11-16 | 中国神华能源股份有限公司 | A kind of method extracting scandium from flyash |
| 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 |
| CN112811468A (en) * | 2020-12-25 | 2021-05-18 | 四川省绵阳市华意达化工有限公司 | Method for improving quality of chromic anhydride |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102249277B (en) | 2013-04-17 |
| CN101838004A (en) | 2010-09-22 |
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Free format text: FORMER OWNER: SHENHUA ZHUNGER ENERGY CO., LTD. Effective date: 20111213 |
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Effective date of registration: 20111213 Address after: 100011 Beijing city Dongcheng District No. 16 Andrew intercontinental 4 storey building Applicant after: China Shenhua Energy Co., Ltd. Address before: 100011 Beijing city Dongcheng District No. 16 Andrew intercontinental 4 storey building Applicant before: China Shenhua Energy Co., Ltd. Co-applicant before: Shenhua Zhunger Energy Co., Ltd. |
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