CN102092751A - Method for preparing aluminum oxide and co-producing hydrochloric acid from aluminum chloride hexahydrate through pyrolytic crystallization - Google Patents
Method for preparing aluminum oxide and co-producing hydrochloric acid from aluminum chloride hexahydrate through pyrolytic crystallization Download PDFInfo
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- CN102092751A CN102092751A CN 201010554860 CN201010554860A CN102092751A CN 102092751 A CN102092751 A CN 102092751A CN 201010554860 CN201010554860 CN 201010554860 CN 201010554860 A CN201010554860 A CN 201010554860A CN 102092751 A CN102092751 A CN 102092751A
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- chloride hexahydrate
- aluminum chloride
- aluminum oxide
- hydrochloric acid
- crystallization
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Abstract
The invention provides a method for preparing aluminum oxide and co-producing hydrochloric acid from crystallized aluminum chloride hexahydrate through pyrolysis crystallization. The method comprises the following steps: sending crystallized aluminum chloride hexahydrate used as a raw material to a pyrolyzing furnace to perform intramolecular dehydration and thermal cracking reaction at 140-900 DEG C and generate the product-aluminum oxide, and using a tail gas treatment system to absorb pyrolytic tail gas and generate the hydrochloric acid byproduct. By adopting the method in the invention, the comprehensive utilization industrial chain of fly ash can be extended, the environmental pollution problem that a lot of fly ash is stored up can be solved, strategic metal resources can be effectively recycled and great economic benefits can be created. The technological process in the invention has the single reactant, concise and clear main process, adequate and stable raw material supply and low production cost; and the emission of three wastes reaches the standard completely, the method in the invention belongs to the comprehensive utilization project of resources and meets the national industrial policy.
Description
Technical field
The present invention relates to a kind ofly the crystallization Aluminum Chloride Hexahydrate at high temperature be decomposed to obtain the method for higher-grade aluminium sesquioxide and by-product hydrochloric acid by calcining.
Background technology
Crystallization Aluminum Chloride Hexahydrate (or claiming crystal aluminum chloride, Aluminum Chloride Hexahydrate) molecular formula is AlCl
36H
2O, a kind of product that obtains for the aluminum chloride aqueous solution condensing crystal, can be used as water treatment agent, casting stiffening agent, wood preservative, paper-making sizing precipitation agent etc., in addition, the crystallization Aluminum Chloride Hexahydrate can be used for also that wool is refining, aluminum hydroxide gel production, the monomeric production of oil chlorination cracking catalyst, polymerize aluminum chloride production and medicine industry etc.
Comprehensive utilization flyash or coal gangue can reclaim wherein the aluminium form with the crystallization Aluminum Chloride Hexahydrate, flyash is to be fuel with the coal, receive the thin ash catch from flue gas, its content accounts for 5%～20% of coal-fired total amount, one of main solid waste of discharging for the coal-burning power plant.
Utilize the research and the production status of the further production derived product of crystallization Aluminum Chloride Hexahydrate mostly to be production polymerize aluminum chloride etc. at present, produce the alumina product that can be used for electrolysis of aluminum and in pertinent literature, rarely have report.
Aluminum oxide (or claiming aluminium sesquioxide, alumina) molecular formula is Al
2O
3, can be used as abrasive, aluminium metallurgy raw material, and be used to make the products such as aluminium hydroxide of crucible, porcelain, refractory materials, hard mass, different crystal forms.
Along with the Application Areas of aluminium and alloy product thereof is increasingly extensive, the situation that supply falls short of demand appears continuing in metallic aluminium market, for the imbalance between supply and demand of alleviating the aluminum metal resource, optimize the structure of production, at different character raw materials, use multiple recovery method, select that product form comprehensive utilization flexibly is various to contain bauxite resource and waste is imperative.
Summary of the invention
The purpose of this invention is to provide the method that a kind of pyrolysis crystallization Aluminum Chloride Hexahydrate is produced aluminum oxide and passed through tail gas absorption system by-product hydrochloric acid.
The production method of aluminum oxide of the present invention and hydrochloric acid comprises the following steps:
(1) AlCl
36H
2O (crystallization Aluminum Chloride Hexahydrate) delivers to the raw material feed bin, by sending into calcining furnace after the metering, temperature of charge reacts 30min～180min down at 140～900 ℃, and thermo-cracking obtains aluminum oxide, hydrogenchloride and water vapour, keep little positive negative pressure in the rotary reaction furnace, force value is controlled at 50～-50mmH
2O.
(2) alumina product is discharged body of heater from the calcining furnace tail, is cooled to 50～120 ℃ through cooling apparatus, sends into subsequent processing or is packaged as the finished product aluminum oxide; Hydrogenchloride that reaction generates and water vapour cool off, absorb the hydrochloric acid of by-product technical grade through dedusting; Do not absorb completely HCl tail gas and enter the absorption that neutralizes of alkali cleaning equipment and sig water, realize qualified discharge.
The main chemical reactions equation is as follows:
2AlCl
3·6H
2O→Al
2O
3+9H
2O+6HCl
HCl+NaOH→NaCl+H
2O
The present invention has extended the industrial chain of total utilization of PCA, has not only solved the problem of environmental pollution that flyash is stored up in a large number, and efficient recovery strategy metal resource, can create huge economic benefit.This technology byproduct hydrochloric acid can reach the technical grade standard, and the reaction acid as Aluminum Chloride Hexahydrate in the flyash refines reaches the resource circulation utilization.
This project technological process reactant is single, main technology simple and clear, and raw material supply is sufficient stable, low production cost, " three wastes " are qualified discharge all, belongs to the comprehensive utilization of resources project, meets the industry policy that country advocates.
Description of drawings
Fig. 1 is the pyrolytic process schema.
Fig. 2 is the vent gas treatment schema.
Embodiment
A kind of pyrolysis crystallization Aluminum Chloride Hexahydrate of the present invention produces aluminum oxide and the embodiment by tail gas absorption system by-product hydrochloric acid comprises:
(1) the crystallization Aluminum Chloride Hexahydrate is delivered to the raw material feed bin, by sending into calcining furnace after the metering.Can select any commercially available prod for use for the material crystal Aluminum Chloride Hexahydrate, preferred, use the total utilization of PCA product; Can select methods well known in the art such as quantitative conveying feeding machine, weightless scale, weighing belt for use for metering method, preferred, use weighing belt to measure; Can select method well known in the art for use for carrying method, preferred, use worm conveyor to carry.
(2) the crystallization Aluminum Chloride Hexahydrate after will measuring is sent into calcining furnace, and temperature of charge is at 140～900 ℃ of reaction 30min～180min down, and thermo-cracking obtains aluminum oxide, hydrogenchloride and water vapour, keeps little positive negative pressure in the rotary reaction furnace, and force value is controlled at 50～-50mmH
2O.For calciner, can select vertical calcining furnace, rotary calcining stove, oscillatory type calcining furnace, tunnel like calcining furnace etc. for use, preferred, use the rotary calcining stove.For the calciner type of heating, can select external-heat or internal heat type for use.
The main chemical reactions equation is as follows:
2AlCl
3·6H
2O→Al
2O
3+9H
2O+6HCl
(3) alumina product is discharged body of heater from the calcining furnace tail, is cooled to 50～120 ℃ through cooling apparatus, sends into subsequent processing or is packaged as the finished product aluminum oxide.The discharging carrying method can be selected method well known in the art for use, and is preferred, uses worm conveyor to carry out discharging.
(4) hydrogenchloride of reaction generation and water vapour are at first removed the dust in the gas, through cooling off and partially absorbing, and after absorbing via two-stage HCl resorber again, by-product hydrochloric acid.For dust removal installation, can select equipment well known in the art such as gravity settling chamber, sack cleaner, electric dust-catching and cleaning equipment for use, preferred, use tornado dust collector or strainer to carry out dedusting; For cooling and absorbing equipment, can select equipment well known in the art for use, preferred, use tower to carry out cooling and absorbing; For follow-up absorption equipment, can select equipment well known in the art for use, preferred, use graphite falling film absorber.
(5) unabsorbed HCl tail gas enters the absorption that neutralizes of alkali cleaning equipment and sig water, realizes qualified discharge.For alkali cleaning equipment, can select equipment well known in the art for use, preferred, use tower; For alkali lye, can select material well known in the art for use, preferred, use sodium hydroxide.
The main chemical reactions equation is as follows:
HCl+NaOH→NaCl+H
2O
There is no particular restriction in the present invention for employed material crystal Aluminum Chloride Hexahydrate, preferentially selects the total utilization of PCA product for use, and the present invention is applicable to any commercially available crystallization Aluminum Chloride Hexahydrate product too.The granularity of Aluminum Chloride Hexahydrate can be 0.2～1.2mm, and the granularity of preferred Aluminum Chloride Hexahydrate is 0.3～0.8mm, and the granularity of preferred Aluminum Chloride Hexahydrate is 0.3～0.5mm.For the purity of Aluminum Chloride Hexahydrate, be preferably 85% or higher, preferred purity is 95% or higher, most preferred purity is 98% or higher.
See also Fig. 1, the crystallization Aluminum Chloride Hexahydrate is sent into and is carried out pyrolysis in the rotary kiln, pyrolysis is temperature required to be provided by hot-air system, hot blast conducts heat by outer wall to be provided heat or directly brings rotary kiln into by the inertia heat-carrying gas in stove, can obtain meeting the alumina product of relevant criterion after the calcining from the stove tail, tail gas send the tail gas absorption system through after the dedusting.
See also Fig. 2, pyrolysis tail gas at first efficiently cools off via the absorption liquid from hydrogenchloride one-level resorber by quenching column and partially absorbs, absorption liquid is sent into the dilute hydrochloric acid storage tank, tail gas enters hydrogenchloride one-level resorber again and is partially absorbed by the absorption liquid from the hydrogenchloride secondary absorber, enter the hydrogenchloride secondary absorber again and partially absorb, enter again finally to enter after scrubber tower is partially absorbed by process water and realize qualified discharge after soda-wash tower is absorbed by alkali lye by absorption liquid from scrubber tower.
Embodiment 1
(1) takes by weighing 40kg crystallization Aluminum Chloride Hexahydrate and deliver to crystallization Aluminum Chloride Hexahydrate feed bin through handling equipment, in feed bin, powder material is entered in the weighing belt after the accurate measurement by valve, send into down in the elephant trunk, send into the feed auger of crystallization Aluminum Chloride Hexahydrate calcining furnace by blanking device, feed auger is sent into material in the crystallization Aluminum Chloride Hexahydrate calcining furnace and is calcined.
Material crystal Aluminum Chloride Hexahydrate bulk density is 0.819g/cm
3, particle size range 0.6～1.2mm, main chemical constitution is as shown in the table:
| Component | AlCl 3.6H 2O | KCl | NaCl | CaCl 2.2H 2O | H 2O |
| Content | 93～95％ | 0.05～0.1％ | 0.05～0.1％ | 0.1～0.5％ | 3～5％ |
(2) the calcining furnace type of heating is taked external-heat, and outside hot blast temperature is controlled between 850～1050 ℃, and temperature of charge is at 650～850 ℃ in the stove.Dehydration and heat scission reaction in the crystallization Aluminum Chloride Hexahydrate carries out in calcining furnace, the residence time of material in calcining furnace is about 60min, the reaction product aluminum oxide enters the feed box of calcining furnace, by the star-shaped feeder successive aluminum oxide is sent into cooler by elephant trunk, be cooled to about 80 ℃, collect the about 8.42kg of alumina product altogether.
Transformation efficiency through calculating crystallization Aluminum Chloride Hexahydrate is 99.608%, pyrolysis gained alumina product particle size range 178～420 μ m, and bulk density is 0.464g/cm
3.
(3) hydrogen chloride gas and the water vapour that generate of heat scission reaction at first enters tornado dust collector, removes most dust in the gas, and then enters strainer and remove remaining dust.Gas after the dedusting is sent into next operation and is absorbed.
In the whole dust removal process, gas temperature remains on more than 180 ℃, generates hcl corrosion equipment and pipeline to prevent hydrogen chloride gas and water vapour dewfall.Total system pressure maintains-little condition of negative pressure operation down of 200Pa, and the negative pressure of system is provided by the negative-pressure air fan of follow-up system, ensures in the operational process that sour gas does not leak.
(4) calcination system institute heat requirement is all provided by hot air circulating system.Heavy oil directly enters the passage between body of heater and the chuck after fully burning in roasting kiln, body of heater is carried out radiation and convective heating simultaneously.
Embodiment 2
(1) takes by weighing 40kg crystallization Aluminum Chloride Hexahydrate and deliver to crystallization Aluminum Chloride Hexahydrate feed bin through handling equipment, in feed bin, powder material is entered in the weighing belt after the accurate measurement by valve, send into down in the elephant trunk, send into the feed auger of crystallization Aluminum Chloride Hexahydrate calcining furnace by blanking device, feed auger is sent into material in the crystallization Aluminum Chloride Hexahydrate calcining furnace and is calcined.
Material crystal Aluminum Chloride Hexahydrate bulk density is 0.819g/cm
3, particle size range 0.3～0.5mm, main chemical constitution is as shown in the table:
| Component | AlCl 3.6H 2O | KCl | NaCl | CaCl 2.2H 2O | H 2O |
| Content | 93～95％ | 0.05～0.1％ | 0.05～0.1％ | 0.1～0.5％ | 3～5％ |
(2) the Sweet natural gas heat-carrying high-temperature gas that produces that burns in roasting kiln enters in the stove from rotary kiln stove tail, and move to the stokehold, the thermograde that formation is successively decreased from the stove tail to burner, temperature of reaction is controlled between 850～1050 ℃, the crystallization Aluminum Chloride Hexahydrate raw material that enters calcining furnace constantly moves to the body of heater back segment in stove, dehydration and heat scission reaction in carrying out, the residence time of material in calcining furnace is about 70min.The reaction product aluminum oxide enters the feed box of calcining furnace, by the blanking device successive aluminum oxide is sent into cooler by elephant trunk, is cooled to about 70 ℃, collects the about 8.43kg of alumina product altogether.
Transformation efficiency through calculating crystallization Aluminum Chloride Hexahydrate is 99.80%, pyrolysis gained alumina product particle diameter 〉=45 μ m.
(3) hydrogen chloride gas and water vapour that hot blast after temperature reduces and heat scission reaction generate at first enter tornado dust collector, remove most dust in the gas, and then enter strainer and remove remaining dust.Gas after the dedusting is sent into next operation and is absorbed after further removing outer other water-soluble gas of hydrogenchloride.
In the whole dust removal process, gas temperature remains on more than 180 ℃, generates hcl corrosion equipment and pipeline to prevent hydrogen chloride gas and water vapour dewfall.Whole dust-removal system is moved under little condition of negative pressure of-300Pa, and the negative pressure of system is provided by the negative-pressure air fan of follow-up system, ensures in the operational process that sour gas does not leak.
(4) the hot cigarette wind that produces after by Sweet natural gas perfect combustion of calcination system institute heat requirement provides.
More than pyrolysis crystallization Aluminum Chloride Hexahydrate production method of alumina provided by the present invention is described in detail.Used specific case herein principle of the present invention and embodiment are set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
Claims (6)
1. the method that pyrolysis crystallization Aluminum Chloride Hexahydrate is produced aluminum oxide and by-product hydrochloric acid is characterized in that comprising the steps:
(1) the crystallization Aluminum Chloride Hexahydrate is delivered to the raw material feed bin, by sending into calcining furnace after the metering, temperature of charge reacts 30min～180min down at 140～900 ℃, and thermo-cracking obtains aluminum oxide, hydrogenchloride and water vapour, keep little positive negative pressure in the calcining furnace, force value is controlled at 50～-50mmH
2O;
(2) aluminum oxide is discharged body of heater from the calcining furnace tail, is cooled to 50～120 ℃ through cooling apparatus, sends into subsequent processing or is packaged as the finished product aluminum oxide; Hydrogenchloride that reaction generates and water vapour are through dedusting, cooling, absorption, the hydrochloric acid of by-product technical grade; Do not absorb completely HCl tail gas and enter the absorption that neutralizes of alkali cleaning equipment and sig water, realize qualified discharge.
2. a kind of pyrolysis crystallization Aluminum Chloride Hexahydrate according to claim 1 is produced the method for aluminum oxide and by-product hydrochloric acid, it is characterized in that crystallization Aluminum Chloride Hexahydrate raw material particle size scope is 0.2～1.2mm.
3. a kind of pyrolysis crystallization Aluminum Chloride Hexahydrate according to claim 1 is produced the method for aluminum oxide and by-product hydrochloric acid, it is characterized in that crystallization Aluminum Chloride Hexahydrate raw material sources are intermediates or other any satisfactory commercially available prod of flyash or coal gangue comprehensive utilization.
4. a kind of pyrolysis crystallization Aluminum Chloride Hexahydrate according to claim 1 is produced the method for aluminum oxide and by-product hydrochloric acid, it is characterized in that the calcining furnace form can be divided into vertical calcining furnace, rotary calcining stove, oscillatory type calcining furnace, tunnel like calcining furnace or other type of furnace.
5. a kind of pyrolysis crystallization Aluminum Chloride Hexahydrate according to claim 1 is produced the method for aluminum oxide and by-product hydrochloric acid, it is characterized in that the calcining furnace type of heating can select to adopt thermal source directly to contact with material with material indirect contact heat supply or thermal source.
6. a kind of pyrolysis crystallization Aluminum Chloride Hexahydrate according to claim 1 is produced the method for aluminum oxide and by-product hydrochloric acid, it is characterized in that calcining temperature is 600～850 ℃.
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| CN104058436A (en) * | 2014-06-12 | 2014-09-24 | 北京航天动力研究所 | Device and method for preparing aluminum oxide by roasting crystalline aluminum chloride hexahydrate in rotary kiln |
| CN104730210A (en) * | 2013-12-24 | 2015-06-24 | 贵阳铝镁设计研究院有限公司 | Testing device for extracting aluminum oxide from aluminum chloride crystal |
| CN105084400A (en) * | 2015-09-18 | 2015-11-25 | 东北大学 | Device and method for preparing activated aluminum oxide |
| CN106241845A (en) * | 2016-08-29 | 2016-12-21 | 何顺爱 | A kind of novel ultrapure ball-aluminium oxide powder preparation method |
| CN108002416A (en) * | 2017-11-27 | 2018-05-08 | 沈阳东大东科干燥煅烧工程技术有限公司 | A kind of drying and calcining processing technology and equipment for crystallizing Aluminum Chloride Hexahydrate |
| CN108862344A (en) * | 2018-07-27 | 2018-11-23 | 东北大学 | A kind of method of the crystal aluminum chloride preparing alumina by hydrolysis of controllable crystal form |
| CN109607587A (en) * | 2019-01-31 | 2019-04-12 | 鲍君杰 | A kind of manufacturing equipment and manufacturing method of ultrafine aluminium hydroxide |
| CN111204784A (en) * | 2020-01-20 | 2020-05-29 | 东北大学 | Method and device for deep hydrolysis and dechlorination of crystalline aluminum chloride |
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| CN114341057A (en) * | 2019-06-07 | 2022-04-12 | 美卓奥图泰芬兰有限公司 | Method and apparatus for thermal decomposition of aluminium chloride hydrate to aluminium oxide |
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| CN104730210A (en) * | 2013-12-24 | 2015-06-24 | 贵阳铝镁设计研究院有限公司 | Testing device for extracting aluminum oxide from aluminum chloride crystal |
| CN104058436A (en) * | 2014-06-12 | 2014-09-24 | 北京航天动力研究所 | Device and method for preparing aluminum oxide by roasting crystalline aluminum chloride hexahydrate in rotary kiln |
| CN105084400A (en) * | 2015-09-18 | 2015-11-25 | 东北大学 | Device and method for preparing activated aluminum oxide |
| CN106241845A (en) * | 2016-08-29 | 2016-12-21 | 何顺爱 | A kind of novel ultrapure ball-aluminium oxide powder preparation method |
| CN106241845B (en) * | 2016-08-29 | 2017-12-22 | 何顺爱 | A kind of ultrapure ball-aluminium oxide powder preparation method |
| CN108002416A (en) * | 2017-11-27 | 2018-05-08 | 沈阳东大东科干燥煅烧工程技术有限公司 | A kind of drying and calcining processing technology and equipment for crystallizing Aluminum Chloride Hexahydrate |
| CN108862344A (en) * | 2018-07-27 | 2018-11-23 | 东北大学 | A kind of method of the crystal aluminum chloride preparing alumina by hydrolysis of controllable crystal form |
| CN109607587A (en) * | 2019-01-31 | 2019-04-12 | 鲍君杰 | A kind of manufacturing equipment and manufacturing method of ultrafine aluminium hydroxide |
| CN114341057A (en) * | 2019-06-07 | 2022-04-12 | 美卓奥图泰芬兰有限公司 | Method and apparatus for thermal decomposition of aluminium chloride hydrate to aluminium oxide |
| CN114341057B (en) * | 2019-06-07 | 2023-11-10 | 美卓奥图泰芬兰有限公司 | Method and apparatus for thermal decomposition of aluminum chloride hydrate to aluminum oxide |
| CN111204784A (en) * | 2020-01-20 | 2020-05-29 | 东北大学 | Method and device for deep hydrolysis and dechlorination of crystalline aluminum chloride |
| CN111204784B (en) * | 2020-01-20 | 2021-11-30 | 东北大学 | Method and device for deep hydrolysis and dechlorination of crystalline aluminum chloride |
| CN111453752A (en) * | 2020-06-09 | 2020-07-28 | 孙雪梅 | High-purity alumina and preparation method thereof |
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