CN104671270A - Anhydrous aluminum chloride preparation method - Google Patents
Anhydrous aluminum chloride preparation method Download PDFInfo
- Publication number
- CN104671270A CN104671270A CN201310610471.XA CN201310610471A CN104671270A CN 104671270 A CN104671270 A CN 104671270A CN 201310610471 A CN201310610471 A CN 201310610471A CN 104671270 A CN104671270 A CN 104671270A
- Authority
- CN
- China
- Prior art keywords
- aluminum chloride
- crystal
- gas
- anhydrous
- hydrochloric acid
- 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.)
- Pending
Links
Abstract
The present invention discloses an anhydrous aluminum chloride preparation method, which comprises: using fly ash or aluminum-containing ore with an aluminum content of more than 30% as a raw material, carrying out dissolution with hydrochloric acid to obtain an aluminum chloride solution, carrying out concentration crystallization to obtain the aluminum chloride crystal, mixing the aluminum chloride crystal and solid carbon, placing into a chlorination furnace with a temperature of higher than 300 DEG C and a pressure of normal pressure or slightly negative pressure, introducing chlorine gas to generate anhydrous aluminum chloride mixing gas with a mass percentage of more than 10%, and carrying out refining impurity-removing to obtain the anhydrous aluminum chloride with the purity of more than or equal to 99%. The method of the invention has characteristics of readily available and inexpensive raw materials, low energy source consumption, simple process, easy industrial large-scale production, and the like.
Description
Technical field
the present invention relates to a kind of preparation method of Aluminum chloride anhydrous, belong to Technology of Comprehensive Utilization of Coal Ash field.
Background technology
aluminum chloride, molecular formula AlCl3, English name Aluminum trichloride, density 2.44, acid attack product danger label 20, aluminum trichloride (anhydrous) belongs to organic Chemicals, is the main raw material producing dyestuff, be widely used in the preparation of the synthesis of catalyzer, petroleum cracking, synthetic dyestuff, rubber, medicine, washing composition, spices, agricultural chemicals and organo-aluminium compound, also for the aspect such as processing of Metal smelting and wetting oil.In recent years, along with the exhaustion day by day of global bauxite resource, the production cost of Aluminum chloride anhydrous progressively reduces, and it most possibly becomes the raw material sources that replacement aluminum oxide becomes electrolytic aluminum.The great advantage of aluminum chloride electrolysis aluminium metallurgy is that energy consumption is low, ton aluminium power consumption 9000 ~ 10000KWh, and anode does not consume, and chlorine also can be accomplished to recycle.
current Aluminum chloride anhydrous preparation mainly contains two kinds of technology.One is aluminium ingot method, namely adopts chlorine directly by molten metal aluminium, and make both directly contact and produce, its reaction formula is:, the feature of aluminium ingot method is that technical process is simple, and equipment is few, invests low, but owing to adopting metallic aluminium higher as raw materials cost.Another kind is alundum method, namely adopts aluminum oxide, chlorine and carbon as raw material, and at a certain temperature, three jointly reacts and produces, and its reaction formula is:, wherein m+2n=3.The feature of alundum method is that cost of material is low, and cost is much lower than aluminium ingot method, but comprehensive cost or higher.
Summary of the invention
the object of the invention is to, a kind of preparation method of Aluminum chloride anhydrous is provided.Take flyash as raw material production Aluminum chloride anhydrous, for the preparation of Aluminum chloride anhydrous in aluminum chloride fused salt electrolysis process production metallic aluminium provides, a kind of energy consumption is little, technique is simple, production cost is low, is applicable to the preparation method that industrial large-sizedization is produced.
technical scheme of the present invention:
a preparation method for Aluminum chloride anhydrous, the method flyash or containing aluminium be greater than 30% containing aluminium ore be raw material, obtain liquor alumini chloridi with hydrochloric acid stripping; Crystal aluminum chloride is obtained through condensing crystal; Put into temperature after being mixed with solid carbon by crystal aluminum chloride higher than 300 DEG C, pressure is pass into chlorine in the chlorination furnace of normal pressure or tiny structure, generates the Aluminum chloride anhydrous that mass percentage is greater than 10%.
in preceding method, the liquor alumini chloridi of described hydrochloric acid stripping carries out stripping in electrically heated retort, with constant feeder, raw material is slowly added in hydrochloric acid, control leaching condition: hydrochloric acid and material molar ratio are greater than 6.5, pressure is greater than 0.5Mpa, temperature for being greater than 100 DEG C.
in preceding method, described condensing crystal is: liquor alumini chloridi is placed on evaporation concentration in evaporative crystallization tank.
in preceding method, described solid carbon is refinery coke, gac, charcoal, coal tar or calcined coke.
in preceding method, the chlorine in described chlorination furnace and the mol ratio of crystal aluminum chloride are greater than 6.5; Solid carbon in chlorination furnace and the mol ratio of crystal aluminum chloride are greater than 6.5.
in preceding method, the Aluminum chloride anhydrous that described mass percentage is greater than 10% obtains through refining and edulcoration the Aluminum chloride anhydrous that purity is greater than 95%.
in preceding method, described purity be 95% Aluminum chloride anhydrous be warming up to more than 178 DEG C the purity Aluminum chloride anhydrouss that are greater than 99%.
in preceding method, described refining and edulcoration is separated according to the boiling-point difference of gas after chlorination, adopts three grades of condensation method of purifications; The first step keeps condensing temperature to be 280 ± 10 DEG C, the FeCl3 gas of condense most; The second stage keeps condensing temperature to be 260 ± 5 DEG C, the FeCl3 gas of condensation of residual and the AlCl3 gas of trace; The third stage keeps condensing temperature to be 160 ± 2 DEG C, total condensation AlCl3 gas and obtain the Aluminum chloride anhydrous that purity is greater than 95%.
in preceding method, the tail gas of described refining and edulcoration discharge contains CO, CO2, HCl, Cl2, passes into after alkaline solution absorbs remaining HCl and Cl2 again and discharge after water absorption HCl and a part of Cl2.
compared with prior art, the technology that the present invention adopts has that raw material is cheap and easy to get, energy consumption is few, technique is simple, be easy to the features such as industrial large-sizedization production.Because These characteristics the present invention can reduce the production cost of Aluminum chloride anhydrous greatly, be particularly useful for the preparation that aluminum chloride fused salt electrolysis process produces Aluminum chloride anhydrous in metallic aluminium.
Embodiment
below in conjunction with embodiment, the present invention is described in further detail, but not as any limitation of the invention.
a preparation method for Aluminum chloride anhydrous, with flyash or containing aluminium be greater than 30% containing aluminium ore (as bauxite, coal gangue etc.) be raw material, obtain liquor alumini chloridi with hydrochloric acid stripping; Crystal aluminum chloride is obtained through condensing crystal; By crystal aluminum chloride and solid carbon (as refinery coke, gac, charcoal, coal tar, calcined coke etc.) with constant feeder by solid carbon and the mol ratio of crystal aluminum chloride be greater than 6.5 mix after add temperature higher than 300 DEG C, pressure is in the chlorination furnace of normal pressure or tiny structure, the ratio being greater than 6.5 in the mol ratio of chlorine and crystal aluminum chloride passes into chlorine, generates the Aluminum chloride anhydrous that mass percentage is greater than 10% after raw material and solid carbon react in chlorination furnace.If obtain the Aluminum chloride anhydrous that purity is higher, can also obtain through refining and edulcoration the Aluminum chloride anhydrous that purity is greater than 95%.Again the Aluminum chloride anhydrous of 95% is heated to more than the 178 DEG C Aluminum chloride anhydrouss that also can obtain purity and be greater than 99%.
aforementioned hydrochloric acid stripping obtains liquor alumini chloridi and is: in electrically heated retort, carry out stripping, is slowly added in hydrochloric acid by raw material with constant feeder, controls leaching condition: hydrochloric acid and material molar ratio are greater than 6, pressure is greater than 0.5Mpa, temperature is greater than 100 DEG C.Aforementioned condensing crystal is: liquor alumini chloridi is placed on evaporation concentration in evaporative crystallization tank.
the gas that chlorination reaction and refining and edulcoration process generate has AlCl3, FeCl3, CO, CO2, HCl, Cl2 etc., and slag mainly contains: MgCl2, CaCl2, NaCl, KCl.Slag periodic exhaustion, furnace gas collects FeCl3, AlCl3 by three grades of coolings.The first step keeps condensing temperature to be 280 ± 10 DEG C; The second stage keeps condensing temperature to be 260 ± 5 DEG C; The third stage keeps condensing temperature to be 160 ± 2 DEG C.Other tail gas enter air after being absorbed by water again after alkali liquor absorption.
Embodiment: electrically heated retort, constant feeder is adopted slowly to add in the hydrochloric acid soln of 3600g 30% by 1000g flyash solid, control stripping pressure 0.5Mpa, temperature is 150 DEG C, hydrochloric acid stripping is carried out to flyash, obtain impure more liquor alumini chloridi, the liquor alumini chloridi evaporative crystallization tank condensing crystal that reaction generates obtains crystal aluminum chloride 2013g, mix with the refinery coke of 700g carbon containing 98.5%, add chlorination furnace with constant feeder to pass into 4270g chlorine and react, controlling chlorination reaction temperature is 400 DEG C, chlorination reaction generates the AlCl3 mixed gas 7360g of 13.6%, its gaseous species has AlCl3, FeCl3, CO, CO2, HCl, Cl2 etc., slag mainly contains: MgCl2, CaCl2, NaCl, KCl.Slag periodic exhaustion, furnace gas collects the aluminum trichloride (anhydrous) 1033g of 95% by three grades of condensation refining and edulcorations.Again the Aluminum chloride anhydrous of 95% is heated to 182 DEG C of distillation condensations and collects the aluminum trichloride (anhydrous) 1023g obtaining 99%, after its tail gas CO, CO2, HCl, Cl2 are absorbed by water, after alkali liquor absorption, enter air again.
Claims (9)
1. a preparation method for Aluminum chloride anhydrous, is characterized in that: the method flyash or containing aluminium be greater than 30% containing aluminium ore be raw material, obtain liquor alumini chloridi with hydrochloric acid stripping; Crystal aluminum chloride is obtained through condensing crystal; Put into temperature after being mixed with solid carbon by crystal aluminum chloride higher than 300 DEG C, pressure is pass into chlorine in the chlorination furnace of normal pressure or tiny structure, generates the Aluminum chloride anhydrous that mass percentage is greater than 10%.
2. method according to claim 1, it is characterized in that: the liquor alumini chloridi of described hydrochloric acid stripping carries out stripping in electrically heated retort, with constant feeder, raw material is slowly added in hydrochloric acid, control leaching condition: hydrochloric acid and material molar ratio are greater than 6.5, pressure is greater than 0.5Mpa, temperature for being greater than 100 DEG C.
3. method according to claim 1, is characterized in that: described condensing crystal is: liquor alumini chloridi is placed on evaporation concentration in evaporative crystallization tank.
4. method according to claim 1, is characterized in that: described solid carbon is refinery coke, gac, charcoal, coal tar or calcined coke.
5. method according to claim 1, is characterized in that: the chlorine in described chlorination furnace and the mol ratio of crystal aluminum chloride are greater than 6.5; Solid carbon in chlorination furnace and the mol ratio of crystal aluminum chloride are greater than 6.5.
6. method according to claim 1, is characterized in that: the Aluminum chloride anhydrous that described mass percentage is greater than 10% obtains through refining and edulcoration the Aluminum chloride anhydrous that purity is greater than 95%.
7. method according to claim 6, is characterized in that: described purity be 95% Aluminum chloride anhydrous be warming up to more than 178 DEG C the purity Aluminum chloride anhydrouss that are greater than 99%.
8. method according to claim 6, is characterized in that: described refining and edulcoration is separated according to the boiling-point difference of gas after chlorination, adopts three grades of condensation method of purifications; The first step keeps condensing temperature to be 280 ± 10 DEG C, the FeCl3 gas of condense most; The second stage keeps condensing temperature to be 260 ± 5 DEG C, the FeCl3 gas of condensation of residual and the AlCl3 gas of trace; The third stage keeps condensing temperature to be 160 ± 2 DEG C, total condensation AlCl3 gas and obtain the Aluminum chloride anhydrous that purity is greater than 95%.
9. method according to claim 6, is characterized in that: the tail gas of described refining and edulcoration discharge contains CO, CO2, HCl, Cl2, absorbs to pass into after alkaline solution absorbs remaining HCl and Cl2 after HCl and a part of Cl2 again discharge through water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310610471.XA CN104671270A (en) | 2013-11-27 | 2013-11-27 | Anhydrous aluminum chloride preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310610471.XA CN104671270A (en) | 2013-11-27 | 2013-11-27 | Anhydrous aluminum chloride preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104671270A true CN104671270A (en) | 2015-06-03 |
Family
ID=53306934
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310610471.XA Pending CN104671270A (en) | 2013-11-27 | 2013-11-27 | Anhydrous aluminum chloride preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104671270A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105174297A (en) * | 2015-09-23 | 2015-12-23 | 江苏多伦化工有限公司 | Method for preparing aluminum chloride based on aluminum oxide |
| CN105439179A (en) * | 2015-12-16 | 2016-03-30 | 衢州市远方化工厂（普通合伙） | Method for reducing content of ferric trichloride in anhydrous aluminum trichloride |
| CN105776294A (en) * | 2016-04-06 | 2016-07-20 | 衢州信步化工科技有限公司 | Efficient and energy-saving aluminum trichloride production method |
| CN112374516A (en) * | 2020-11-19 | 2021-02-19 | 衡阳鸿宇化工有限责任公司 | Evaporation concentration crystallization device of aluminum trichloride solution and use method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1482064A (en) * | 2002-09-10 | 2004-03-17 | 章浩龙 | Method of preparing anhydrous aluminium chloride |
| JP3528424B2 (en) * | 1996-05-09 | 2004-05-17 | 日本軽金属株式会社 | Method for producing high-purity anhydrous aluminum chloride |
-
2013
- 2013-11-27 CN CN201310610471.XA patent/CN104671270A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3528424B2 (en) * | 1996-05-09 | 2004-05-17 | 日本軽金属株式会社 | Method for producing high-purity anhydrous aluminum chloride |
| CN1482064A (en) * | 2002-09-10 | 2004-03-17 | 章浩龙 | Method of preparing anhydrous aluminium chloride |
Non-Patent Citations (1)
| Title |
|---|
| 马家玉等: ""高铝粉煤灰氯化法生产无水氯化铝新工艺"", 《有色金属（冶炼部分）》, no. 10, 31 October 2013 (2013-10-31) * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105174297A (en) * | 2015-09-23 | 2015-12-23 | 江苏多伦化工有限公司 | Method for preparing aluminum chloride based on aluminum oxide |
| CN105439179A (en) * | 2015-12-16 | 2016-03-30 | 衢州市远方化工厂（普通合伙） | Method for reducing content of ferric trichloride in anhydrous aluminum trichloride |
| CN105439179B (en) * | 2015-12-16 | 2017-12-01 | 衢州市远方化工厂（普通合伙） | A kind of method of ferric trichloride content in reduction aluminum trichloride (anhydrous) |
| CN105776294A (en) * | 2016-04-06 | 2016-07-20 | 衢州信步化工科技有限公司 | Efficient and energy-saving aluminum trichloride production method |
| CN105776294B (en) * | 2016-04-06 | 2018-01-30 | 衢州信步化工科技有限公司 | A kind of energy-efficient alchlor production method |
| CN112374516A (en) * | 2020-11-19 | 2021-02-19 | 衡阳鸿宇化工有限责任公司 | Evaporation concentration crystallization device of aluminum trichloride solution and use method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP2800726B1 (en) | A process for manufacturing aluminum from bauxite or its residue | |
| AU2018227891B2 (en) | Method for producing lithium hydroxide from lithium-containing ore | |
| CN103964480A (en) | Process for producing aluminum oxide by using hydrochloric acid method | |
| CN103298742A (en) | Process for manufacturing lower chlorides of titanium | |
| KR20170041701A (en) | Hydrometallurgical process to produce pure magnesium metal and various by-products | |
| CN104671270A (en) | Anhydrous aluminum chloride preparation method | |
| JP6099167B2 (en) | Zinc production method using electric furnace dust as raw material | |
| CN103936047B (en) | A kind of preparation method of anhydrous Aluminum chloride | |
| CN104773746A (en) | Anhydrous aluminum chloride production method | |
| CN111321425B (en) | Molten salt chlorination TiCl production4Comprehensive recycling method of discharged waste salt | |
| CN103241751A (en) | Preparation method for high-purity magnesium oxide | |
| CN102817041A (en) | Method for preparing magnesium hydroxide, magnesium and magnesium aluminate spinel by bischofite | |
| US9920398B2 (en) | Zinc production method | |
| CN104340994B (en) | A kind of method of CFBB total utilization of PCA | |
| CN101555028A (en) | Method for preparing high purity anhydrous magnesium chloride by gas-solid reaction | |
| Wulandari et al. | Magnesium: current and alternative production routes | |
| CN110494574A (en) | The method that lithium hydroxide is prepared by the ore containing lithium by chlorination and chloralkali process | |
| CN104313641A (en) | Method for producing metal aluminum or aluminum magnesium alloy from low grade bauxite | |
| CN105386082B (en) | A kind of preparation method of magnesium metal | |
| CN111039304A (en) | Method for preparing ammonium sulfate and sodium bicarbonate by using sodium sulfate | |
| CN104556156A (en) | Preparation method of anhydrous magnesium chloride | |
| CN101318680B (en) | Process for preparing kryocide | |
| CN103374662B (en) | Device for recycling waste residues containing barium comprehensively during refined aluminum production process | |
| CN202626267U (en) | Equipment for comprehensively recycling barium-containing waste residues produced in production process of refined aluminum | |
| CN113104870B (en) | Continuous preparation method of molten salt electrolyte for electrolytic magnesium |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150603 |