CN103626215B - Method and device for preparing aluminum trichloride - Google Patents
Method and device for preparing aluminum trichloride Download PDFInfo
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- CN103626215B CN103626215B CN201310422231.7A CN201310422231A CN103626215B CN 103626215 B CN103626215 B CN 103626215B CN 201310422231 A CN201310422231 A CN 201310422231A CN 103626215 B CN103626215 B CN 103626215B
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Abstract
The invention provides a method and a device for preparing aluminum trichloride. The method comprises the following steps: preheating a circulation gas to be 300-500 DEG C outside a furnace; mixing the preheated circulation gas with chlorine, subsequently feeding into a fluidized reactor, enabling the gas to move from bottom to top inside the fluidized reactor, and stopping feeding the circulation gas when the fluidized reactor is full of the gas and the gas is returned to the furnace through a return pipeline connected with a gas outlet in the top of the fluidized reactor; pressurizing the gas through a pressurization unit arranged outside the fluidized reactor so as to form a fluidized flow field inside the fluidized reactor; adding aluminum powder into the fluidized reactor to be in countercurrent contact and reacted with chlorine and the circulation gas so as to generate an aluminum trichloride gas; splitting the gas discharged from the gas outlet into a first branch flow and a second branch flow, cooling down the first branch flow, collecting aluminum trichloride in the first branch flow, feeding back the first branch flow to the furnace, and directly feeding back the second branch flow to the furnace. The method is capable of continuously preparing aluminum trichloride, and has the advantages that the temperature in the preparation process is low, chlorine can be recycled, the heat can be supplied by self, the purity of a product is high, and the like.
Description
Technical field
The present invention relates to the preparation field of aluminum chloride, more particularly, relate to one and produce aluminum chloride method and device with fluidized regime.
Background technology
Aluminum chloride is widely used in medicine, agricultural chemicals, dyestuff, spices, metallurgy, plastics, lubrication wet goods industry, is important inorganic chemical product, main catalyzer, the washing composition, by force dewatering agent, titanium dioxide nucleator etc. being used as organic synthesis.
Current industrial aluminum trichloride (anhydrous) preparation method divides two classes: first kind metallic aluminium chlorination process, and metallic aluminium is put into airtight chlorination reaction stove, logical chlorine carries out chlorination reaction, the aluminum chloride sublimation generated enters trap, through trapping, i.e. obtained aluminum chloride finished product, net reaction 2Al+3Cl
2→ 2AlCl
3.Current domestic aluminum chloride production technique almost all adopts the aluminium ingot method in metallic aluminium chlorination process, namely chlorine passes into the aluminium ingot rising through melting in stove with the form of bubble bottom Reaktionsofen, gas-liquid contact reaction generates aluminum chloride (gas phase), and temperature of reaction controls at about 800 DEG C.When aluminium ingot method shortcoming is that chlorine is reacted by aluminium ingot, in the relatively excessive therefore reaction product of aluminium, there are monochlor(in)ate aluminium and al dichloride.
Equations of The Second Kind alundum method, this method jointly reacts with aluminum oxide, chlorine and carbon three to produce.The gas-phase product generated removes trap through precooling, purification, obtained aluminum chloride finished product.Net reaction Al
2o
3+ (m+n) C+3Cl
2→ 2AlCl
3+ mCO+nCO
2.Alundum method is high to aluminum oxide purity requirement, and the CO in addition in reaction end gas needs oxidation further.Therefore alundum method domestic industry adopts hardly.
Summary of the invention
For the deficiencies in the prior art, an object of the present invention is to solve in above-mentioned prior art the one or more problems existed.
To achieve these goals, an aspect of of the present present invention provides a kind of method preparing aluminum chloride.Described method is aluminium powder and chlorine are reacted to generate aluminum chloride in 300 ~ 500 DEG C of fluidization flow fields, wherein, described 300 ~ 500 DEG C of fluidization flow fields are formed by circulation gas fluidisation, described circulation gas be not with reactive aluminum and liquefaction temperature lower than the gas of the liquefaction temperature of aluminum chloride and/or aluminum chloride gas.
According to the embodiment preparing the method for aluminum chloride of the present invention, said method comprising the steps of: in outer warm-up cycle gas to 300 ~ 500 DEG C of fluidization Reaktionsofen; Pass into after circulation gas after preheating is mixed with chlorine in fluidization Reaktionsofen, gas moves from bottom to top in the body of heater of fluidization Reaktionsofen, when gas is full of body of heater and is returned in body of heater by the reflux line be connected with the furnace roof air outlet of fluidization Reaktionsofen, stop passing into circulation gas; By the presser unit be arranged on outside fluidization Reaktionsofen, described gas is pressurizeed, to make to form fluidization flow field in stove; Add aluminium powder, aluminium powder also reacts with chlorine and circulation gas counter current contact in fluidization Reaktionsofen produces aluminum chloride gas; After shunting, form the first tributary and the second tributary from described air outlet expellant gas, the gas wherein in the first tributary returns in stove after cooling and collect aluminum chloride, and the gas in the second tributary directly returns in stove.
According to the embodiment preparing the method for aluminum chloride of the present invention, the gas in the first tributary account for from the volumn concentration of air outlet expellant gas be 6% ~ 50%.
According to the embodiment preparing the method for aluminum chloride of the present invention, described not with reactive aluminum and liquefaction temperature is one or more in nitrogen, helium and argon gas lower than the gas of the liquefaction temperature of aluminum chloride.
According to the embodiment preparing the method for aluminum chloride of the present invention, the mass ratio of described chlorine and described aluminium powder is 3.94 ~ 5.00:1.
According to the embodiment preparing the method for aluminum chloride of the present invention, the volume ratio of described circulation gas and described chlorine is 1 ~ 11:1.
Another aspect provides a kind of device preparing aluminum chloride.Described device comprises fluidization Reaktionsofen, dosage unit, air supply unit, presser unit, dividing cell and cooling and collector unit, wherein, the fluidization Reaktionsofen charging opening that comprises body of heater, be arranged on the inlet mouth of bottom of furnace body, be arranged on the air outlet at body of heater top and be arranged in the middle part of body of heater on sidewall; Dosage unit is connected to add aluminium powder in fluidization Reaktionsofen with described charging opening; Air supply unit is connected to pass into chlorine and circulation gas in fluidization Reaktionsofen with described inlet mouth; Dividing cell is connected with described air outlet and will be divided into the first tributary and the second tributary from air outlet expellant gas, wherein, first tributary, cooling and collector unit, presser unit are connected to form the first loop with fluidization Reaktionsofen successively, and the second tributary, presser unit are connected to form second servo loop with fluidization Reaktionsofen successively; Cooling and collector unit are for cooling and the aluminum chloride collected in gas control the temperature of reaction system; Presser unit is used for pressurizeing to make to form fluidization flow field in fluidization Reaktionsofen to the gas in the first tributary and the second tributary.
Compared with prior art, the present invention can continuous production aluminum chloride, and has that preparation process temperature is low, chlorine is able to recycle, heat is self-sufficient, obtained aluminum chloride product purity advantages of higher.
Accompanying drawing explanation
By the description carried out below in conjunction with accompanying drawing, above and other object of the present invention and feature will become apparent, wherein:
Fig. 1 is the schematic diagram preparing the device of aluminum chloride of exemplary embodiment of the present.
Description of reference numerals:
10, Reaktionsofen 20, dosage unit 30, air supply unit 40, presser unit 50, tributary 60, dividing cell 51, first tributary 52, second, cooling and collector unit.
Embodiment
Hereinafter, will describe in detail with exemplary embodiment by reference to the accompanying drawings according to method and the device of preparing aluminum chloride of the present invention.
The method preparing aluminum chloride according to an aspect of the present invention, its major technique thinking is aluminium powder and chlorine are reacted to generate aluminum chloride in 300 ~ 500 DEG C of fluidization flow fields, wherein, described 300 ~ 500 DEG C of fluidization flow fields are formed by circulation gas fluidisation, described circulation gas be not with reactive aluminum and liquefaction temperature lower than the gas of the liquefaction temperature of aluminum chloride and/or aluminum chloride gas.Wherein, not with reactive aluminum and liquefaction temperature can be one or more in nitrogen, helium and argon gas lower than the gas of the liquefaction temperature of aluminum chloride.
Particularly, in one exemplary embodiment, said method comprising the steps of:
In outer warm-up cycle gas to 300 ~ 500 DEG C of fluidization Reaktionsofen; Pass into after circulation gas after preheating is mixed with chlorine in fluidization Reaktionsofen, gas moves from bottom to top in the body of heater of fluidization Reaktionsofen, when gas is full of body of heater and is returned in body of heater by the reflux line be connected with the furnace roof air outlet of fluidization Reaktionsofen, stop passing into circulation gas; By the presser unit be arranged on outside fluidization Reaktionsofen, described gas is pressurizeed, to make to form fluidization flow field in stove; Continuously add aluminium powder, aluminium powder also reacts with chlorine and circulation gas counter current contact in fluidization Reaktionsofen produces aluminum chloride gas; After shunting, form the first tributary and the second tributary from described air outlet expellant gas, the gas wherein in the first tributary returns in stove after cooling and collect aluminum chloride, and the gas in the second tributary directly returns in stove.
Because aluminium powder and chlorine reaction release a large amount of heat, this heat enough offsets radiation dispersed heat, therefore external heat is not needed in production process, unnecessary heat is then balanced by the shunting in the first tributary, particularly, gas in first tributary is through overcooling and after collecting aluminum chloride, the tail gas formed returns in stove, the temperature of tail gas is lower than the gas temperature in the second tributary, can heat in balanced reaction process except maintenance Reaktionsofen heat balance after both mixing, can find out, can regulating stove interior reaction temperature from the ratio of air outlet expellant gas by regulating gas in the first tributary to account for.In addition, under the prerequisite ensureing reaction in furnace temperature, the gas proportion in the first tributary is larger, and the rate of recovery of aluminum chloride is higher.Preferably, the gas in the first tributary account for from the volumn concentration of air outlet expellant gas be 6% ~ 50%.
The mass ratio of chlorine and aluminium powder can be 3.94:1 ~ 5.00:1.The volume ratio of chlorine and circulation gas is 1:1 ~ 11:1.In process of production can flexible output, change the add-on of chlorine and corresponding conversion aluminium powder amount, aluminum chloride quantum of output is corresponding to be changed, but circulation gas and chlorine resultant constant.
Fig. 1 is the schematic diagram preparing the device of aluminum chloride of exemplary embodiment of the present.As shown in Figure 1, the device preparing aluminum chloride according to a further aspect of the invention comprises fluidization Reaktionsofen (referred to as Reaktionsofen) 10, dosage unit 20, air supply unit 30, presser unit 40, dividing cell 50 and cooling and collector unit 60.
Wherein, fluidization Reaktionsofen 10 comprise body of heater, the inlet mouth be arranged on bottom of furnace body, the charging opening that is arranged on the air outlet on body of heater top and is arranged in the middle part of body of heater on sidewall.Fluidization Reaktionsofen can adopt fluidization Reaktionsofen conventional in prior art or reactor, does not repeat them here.
Dosage unit 20 is connected to add aluminium powder in fluidization Reaktionsofen with charging opening.
Air supply unit 30 is connected to pass into chlorine and circulation gas in fluidization Reaktionsofen with inlet mouth.
Dividing cell 50 is connected with described air outlet and will be divided into the first tributary 51 and the second tributary 52 from air outlet expellant gas, wherein, first tributary 51, cooling and collector unit 60, presser unit 40 are connected to form the first loop with fluidization Reaktionsofen 10 successively, and the second tributary 52, presser unit 40 are connected to form second servo loop with fluidization Reaktionsofen 10 successively.Dividing cell can adopt has an import, two outlet T-valve, but the present invention is not limited thereto, as long as dividing cell can realize shunting action.
Cooling and collector unit 60 are for cooling and the aluminum chloride collected in gas control the temperature of reaction system.Such as, when reaction in furnace system temperature is higher than 500 DEG C, increase the gas flow entering the first tributary 51, reduce gas and enter the flow in the second tributary 52, the gas in the first tributary 51 to return after cooling in Reaktionsofen and balances heat unnecessary in stove in cooling and collector unit 60 together with the gas in the second tributary 52.
Presser unit 40 makes to form fluidization flow field in fluidization Reaktionsofen for pressurizeing the gas in the first tributary and the second tributary.
Connected by pipeline between each parts and each pipeline be provided with at least one valve (such as flow valve), and the resistance to air loss of complete assembly is better.It should be noted that, when circulation gas is aluminum chloride, must shunt from air outlet expellant gas, otherwise, to be almost all liquefied collection as the aluminum chloride of circulation gas after overcooling and collector unit; When circulation gas is other gases, can carry out shunting also can not shunting, correspondingly operation can realize by regulating the valve on each pipeline.
In order to understand above-mentioned exemplary embodiment of the present invention better, below in conjunction with concrete example, it is further described.
Example 1
Outside Reaktionsofen, nitrogen is preheated to 300 DEG C; Pass into after nitrogen after preheating is mixed with chlorine in fluidization Reaktionsofen, the volume ratio 1:1 of nitrogen and chlorine, gas moves from bottom to top in body of heater, when gas is full of body of heater and is returned in stove by the reflux line be connected with furnace roof air outlet, stops passing into nitrogen; By the presser unit be arranged on outside fluidization Reaktionsofen, gas is pressurizeed, to make to form fluidization flow field in stove; Add aluminium powder from charging opening, the mass ratio of chlorine and aluminium powder is 3.94:1, and aluminium powder also reacts with chlorine and nitrogen counter current contact in Reaktionsofen produces aluminum chloride gas; Reacted gas is discharged rear portion gas and is entered aluminum chloride trap from the first tributary from air outlet, Reaktionsofen is flowed back to after the pressurization of its tail gas, Reaktionsofen is flowed back to after the remaining gas of air outlet discharge flows through direct weighting from second, wherein, the gas in the first tributary account for from the volumn concentration of air outlet expellant gas be 50%.
Example 2
Outer by aluminum chloride air preheat to 500 DEG C at Reaktionsofen; Pass in fluidization Reaktionsofen after aluminum chloride gas after preheating is mixed with chlorine, the volume ratio 11:1 of aluminum chloride gas and chlorine, gas moves from bottom to top in body of heater, when gas is full of body of heater and is returned in stove by the reflux line be connected with furnace roof air outlet, stop passing into aluminum chloride gas; By the presser unit be arranged on outside fluidization Reaktionsofen, gas is pressurizeed, to make to form fluidization flow field in stove; Add aluminium powder from charging opening, the mass ratio of chlorine and aluminium powder is 5.00:1, and aluminium powder contacts with chlorine with aluminum chloride back flow of gas and reacts in Reaktionsofen produces aluminum chloride gas; Reacted gas is discharged rear portion gas and is entered aluminum chloride trap from the first tributary from air outlet, Reaktionsofen is flowed back to after the pressurization of its tail gas, Reaktionsofen is flowed back to after the remaining gas of air outlet discharge flows through direct weighting from second, wherein, the gas in the first tributary account for from the volumn concentration of air outlet expellant gas be 6%.
Example 3
Outer by aluminum chloride air preheat to 400 DEG C at Reaktionsofen; Pass in fluidization Reaktionsofen after aluminum chloride gas after preheating is mixed with chlorine, the volume ratio 5:1 of aluminum chloride gas and chlorine, gas moves from bottom to top in body of heater, when gas is full of body of heater and is returned in stove by the reflux line be connected with furnace roof air outlet, stop passing into aluminum chloride gas; By the presser unit be arranged on outside fluidization Reaktionsofen, gas is pressurizeed, to make to form fluidization flow field in stove; Add aluminium powder from charging opening, the mass ratio of chlorine and aluminium powder is 4.50:1, and aluminium powder contacts with chlorine with aluminum chloride back flow of gas and reacts in Reaktionsofen produces aluminum chloride gas; Reacted gas is discharged rear portion gas and is entered aluminum chloride trap from the first tributary from air outlet, Reaktionsofen is flowed back to after the pressurization of its tail gas, Reaktionsofen is flowed back to after the remaining gas of air outlet discharge flows through direct weighting from second, wherein, the gas in the first tributary account for from the volumn concentration of air outlet expellant gas be 12%.
Example 4
Outside Reaktionsofen, helium is preheated to 350 DEG C; Pass into after helium after preheating is mixed with chlorine in fluidization Reaktionsofen, the volume ratio 7:1 of helium and chlorine, gas moves from bottom to top in body of heater, when gas is full of body of heater and is returned in stove by the reflux line be connected with furnace roof air outlet, stops passing into helium; By the presser unit be arranged on outside fluidization Reaktionsofen, gas is pressurizeed, to make to form fluidization flow field in stove; Add aluminium powder from charging opening, the mass ratio of chlorine and aluminium powder is 4.30:1, and aluminium powder also reacts with chlorine and helium counter current contact in Reaktionsofen produces helium; Reacted gas is discharged rear portion gas and is entered aluminum chloride trap from the first tributary from air outlet, Reaktionsofen is flowed back to after the pressurization of its tail gas, Reaktionsofen is flowed back to after the remaining gas of air outlet discharge flows through direct weighting from second, wherein, the gas in the first tributary account for from the volumn concentration of air outlet expellant gas be 20%.
Can find out, the temperature (800 DEG C) that the present invention prepares temperature of reaction (300 ~ 500 DEG C) the more current Industrial Metal aluminium chlorination process of the method for aluminum chloride is low, and the liquefaction temperature of the circulation gas adopted is lower than the liquefaction temperature of aluminum chloride gas, thus, in the process of collecting aluminum chloride, circulation gas can not be liquefied as liquid, the aluminum chloride purity of preparation is high, color and luster is good, and in addition, chlorine obtains recycle in process of production.
Although above by describing the present invention in conjunction with exemplary embodiment, it will be apparent to those skilled in the art that when not departing from the spirit and scope that claim limits, various amendment and change can be carried out to exemplary embodiment of the present invention.
Claims (6)
1. prepare the method for aluminum chloride for one kind, it is characterized in that, described method is aluminium powder and chlorine are reacted to generate aluminum chloride in 300 ~ 500 DEG C of fluidization flow fields, wherein, described 300 ~ 500 DEG C of fluidization flow fields are formed by circulation gas fluidisation, described circulation gas be not with reactive aluminum and liquefaction temperature lower than the gas of the liquefaction temperature of aluminum chloride and/or aluminum chloride gas;
Said method comprising the steps of:
In outer warm-up cycle gas to 300 ~ 500 DEG C of fluidization Reaktionsofen;
Pass into after circulation gas after preheating is mixed with chlorine in fluidization Reaktionsofen, gas moves from bottom to top in the body of heater of fluidization Reaktionsofen, when gas is full of body of heater and is returned in body of heater by the reflux line be connected with the furnace roof air outlet of fluidization Reaktionsofen, stop passing into circulation gas;
By the presser unit be arranged on outside fluidization Reaktionsofen, described gas is pressurizeed, to make to form fluidization flow field in stove;
Add aluminium powder, aluminium powder also reacts with chlorine and circulation gas counter current contact in fluidization Reaktionsofen produces aluminum chloride gas;
After shunting, form the first tributary and the second tributary from described air outlet expellant gas, the gas wherein in the first tributary returns in stove after cooling and collect aluminum chloride, and the gas in the second tributary directly returns in stove.
2. the method preparing aluminum chloride according to claim 1, is characterized in that, the gas in the first tributary account for from the volumn concentration of air outlet expellant gas be 6% ~ 50%.
3. the method preparing aluminum chloride according to claim 1, is characterized in that, described not with reactive aluminum and liquefaction temperature is one or more in nitrogen, helium and argon gas lower than the gas of the liquefaction temperature of aluminum chloride.
4. the method preparing aluminum chloride according to claim 1, is characterized in that, the mass ratio of described chlorine and described aluminium powder is 3.94 ~ 5.00:1.
5. the method preparing aluminum chloride according to claim 1, is characterized in that, the volume ratio of described circulation gas and described chlorine is 1 ~ 11:1.
6. prepare a device for aluminum chloride, it is characterized in that, described device comprises fluidization Reaktionsofen, dosage unit, air supply unit, presser unit, dividing cell and cooling and collector unit, wherein,
The charging opening that fluidization Reaktionsofen comprises body of heater, is arranged on the inlet mouth of bottom of furnace body, is arranged on the air outlet at body of heater top and is arranged in the middle part of body of heater on sidewall;
Dosage unit is connected to add aluminium powder in fluidization Reaktionsofen with described charging opening;
Air supply unit is connected to pass into chlorine and circulation gas in fluidization Reaktionsofen with described inlet mouth;
Dividing cell is connected with described air outlet and will be divided into the first tributary and the second tributary from air outlet expellant gas, wherein, first tributary, cooling and collector unit, presser unit are connected to form the first loop with fluidization Reaktionsofen successively, and the second tributary, presser unit are connected to form second servo loop with fluidization Reaktionsofen successively;
Cooling and collector unit are for cooling and the aluminum chloride collected in gas control the temperature of reaction system;
Presser unit is used for pressurizeing to make to form fluidization flow field in fluidization Reaktionsofen to the gas in the first tributary and the second tributary.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310422231.7A CN103626215B (en) | 2013-09-17 | 2013-09-17 | Method and device for preparing aluminum trichloride |
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|---|---|---|---|
| CN201310422231.7A CN103626215B (en) | 2013-09-17 | 2013-09-17 | Method and device for preparing aluminum trichloride |
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| CN103626215B true CN103626215B (en) | 2015-04-15 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105439090B (en) * | 2015-12-14 | 2018-02-06 | 株洲冶炼集团股份有限公司 | A kind of device for preparing anhydrous metal chloride |
| CN108675332B (en) * | 2018-06-28 | 2021-01-26 | 攀钢集团钒钛资源股份有限公司 | Preparation device and preparation method of aluminum trichloride |
| CN109942013B (en) * | 2019-05-13 | 2021-06-29 | 湖南恒光科技股份有限公司 | Process for industrially producing aluminum trichloride |
| CN112984782A (en) * | 2021-02-05 | 2021-06-18 | 陕西翼飞航智能科技有限公司 | Based on CO2Carbonate ore production and CO production in plasma hot blast stove2Decomposed gas recovery system and method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3758675A (en) * | 1970-12-23 | 1973-09-11 | Sir Soc Italiana Resine Spa | Process for preparing aluminum trichloride |
| US3812241A (en) * | 1971-04-30 | 1974-05-21 | Sir Soc Italiana Resine Spa | Process for preparing aluminum trichloride |
| CN2743324Y (en) * | 2004-07-23 | 2005-11-30 | 刘长河 | Device for generating aluminium chloride using filling material fluidization bed method |
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2013
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3758675A (en) * | 1970-12-23 | 1973-09-11 | Sir Soc Italiana Resine Spa | Process for preparing aluminum trichloride |
| US3812241A (en) * | 1971-04-30 | 1974-05-21 | Sir Soc Italiana Resine Spa | Process for preparing aluminum trichloride |
| CN2743324Y (en) * | 2004-07-23 | 2005-11-30 | 刘长河 | Device for generating aluminium chloride using filling material fluidization bed method |
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