CN103626215A - Method and device for preparing aluminum trichloride - Google Patents
Method and device for preparing aluminum trichloride Download PDFInfo
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- CN103626215A CN103626215A CN201310422231.7A CN201310422231A CN103626215A CN 103626215 A CN103626215 A CN 103626215A CN 201310422231 A CN201310422231 A CN 201310422231A CN 103626215 A CN103626215 A CN 103626215A
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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 and a kind ofly in fluidization mode, produce aluminum chloride method and device.
Background technology
Aluminum chloride is widely used in medicine, agricultural chemicals, dyestuff, spices, metallurgy, plastics, lubricated wet goods industry, is important inorganic chemical product, mainly as the catalyzer of organic synthesis, washing composition, strong dewatering agent, titanium dioxide nucleator etc.
Current industrial aluminum trichloride (anhydrous) preparation method divides two classes: first kind metallic aluminium chlorination process, metallic aluminium is put into airtight chlorination reaction stove, and logical chlorine carries out chlorination reaction, the aluminum chloride distillation generating enters trap, through trapping, make 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, to be chlorine pass into the form with bubble in stove rises through the aluminium ingot of melting from Reaktionsofen bottom, gas-liquid contact reaction generates aluminum chloride (gas phase), and temperature of reaction is controlled at 800 ℃ of left and right.When aluminium ingot method shortcoming is that chlorine reacts by aluminium ingot, in the relatively excessive so reaction product of aluminium, there are monochlor(in)ate aluminium and al dichloride.
Equations of The Second Kind alundum method, this method is to produce with the common reaction of aluminum oxide, chlorine and carbon three.The gas-phase product generating removes trap through precooling, purification, makes 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 reaction end gas needs further oxidation in addition.Therefore alundum method domestic industry adopts hardly.
Summary of the invention
For the deficiencies in the prior art, one of object of the present invention is to solve the one or more problems that exist in above-mentioned prior art.
To achieve these goals, an aspect of of the present present invention provides a kind of method of preparing aluminum chloride.Described method is aluminium powder to be reacted in 300～500 ℃ of fluidization flow fields with chlorine generate aluminum chloride, wherein, described 300～500 ℃ of fluidization flow fields are formed by circulation gas fluidisation, described circulation gas be not with reactive aluminum and liquefaction temperature gas and/or the aluminum chloride gas lower than the liquefaction temperature of aluminum chloride.
According to an embodiment who prepares the method for aluminum chloride of the present invention, said method comprising the steps of: warm-up cycle gas to 300～500 ℃ outside fluidization Reaktionsofen; After being mixed with chlorine, circulation gas after preheating passes in fluidization Reaktionsofen, gas is motion from bottom to top in the body of heater of fluidization Reaktionsofen, when gas is full of body of heater and when the reflux line that is connected by the furnace roof air outlet with fluidization Reaktionsofen returns in body of heater, stops passing into circulation gas; By the presser unit being arranged on outside fluidization Reaktionsofen, described gas is pressurizeed, so that form fluidization flow field in stove; Add aluminium powder, aluminium powder also reacts and produces aluminum chloride gas with chlorine and circulation gas counter current contact in fluidization Reaktionsofen; From described air outlet expellant gas through shunting after form the first tributary and the second tributary, wherein the gas in the first tributary through cooling and collect aluminum chloride after return in stove, the gas in the second tributary directly returns in stove.
According to an embodiment who prepares the method for aluminum chloride of the present invention, it is 6%～50% that the gas in the first tributary accounts for from the volumn concentration of air outlet expellant gas.
According to an embodiment who prepares the method for aluminum chloride of the present invention, described is not one or more in nitrogen, helium and argon gas with reactive aluminum and liquefaction temperature lower than the gas of the liquefaction temperature of aluminum chloride.
According to an embodiment who prepares 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 an embodiment who prepares 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 of the present invention provides a kind of device of preparing aluminum chloride.Described device comprises fluidization Reaktionsofen, dosage unit, air supply unit, presser unit, dividing cell and cooling and collector unit, wherein, fluidization Reaktionsofen comprise body of heater, be arranged on bottom of furnace body inlet mouth, be arranged on the air outlet at body of heater top and be arranged on the charging opening on the sidewall of body of heater middle part; 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, the first tributary, cooling and collector unit, presser unit are connected to form the first loop successively with fluidization Reaktionsofen, and the second tributary, presser unit are connected to form second servo loop successively with fluidization Reaktionsofen; Cooling and collector unit is for cooling and collect the aluminum chloride of gas and control the temperature of reaction system; Presser unit is for pressurizeing so that 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 the aluminum chloride product purity advantages of higher that preparation process temperature is low, chlorine is able to recycle, heat is self-sufficient, make.
Accompanying drawing explanation
By the description of carrying 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 of the device of preparing 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, dividing cell 51, the first tributary 52, the second tributary 60, cooling and collector unit.
Embodiment
Hereinafter, in connection with accompanying drawing and exemplary embodiment, describe method and the device of preparing aluminum chloride according to of the present invention in detail.
The method of preparing aluminum chloride according to an aspect of the present invention, its major technique thinking is aluminium powder to be reacted in 300～500 ℃ of fluidization flow fields with chlorine generate aluminum chloride, wherein, described 300～500 ℃ of fluidization flow fields are formed by circulation gas fluidisation, described circulation gas be not with reactive aluminum and liquefaction temperature gas and/or the aluminum chloride gas lower than the liquefaction temperature of aluminum chloride.Wherein, lower than the gas of the liquefaction temperature of aluminum chloride, can not be one or more in nitrogen, helium and argon gas with reactive aluminum and liquefaction temperature.
Particularly, in one exemplary embodiment, said method comprising the steps of:
Warm-up cycle gas to 300～500 ℃ outside fluidization Reaktionsofen; After being mixed with chlorine, circulation gas after preheating passes in fluidization Reaktionsofen, gas is motion from bottom to top in the body of heater of fluidization Reaktionsofen, when gas is full of body of heater and when the reflux line that is connected by the furnace roof air outlet with fluidization Reaktionsofen returns in body of heater, stops passing into circulation gas; By the presser unit being arranged on outside fluidization Reaktionsofen, described gas is pressurizeed, so that form fluidization flow field in stove; Continuously add aluminium powder, aluminium powder also reacts and produces aluminum chloride gas with chlorine and circulation gas counter current contact in fluidization Reaktionsofen; From described air outlet expellant gas through shunting after form the first tributary and the second tributary, wherein the gas in the first tributary through cooling and collect aluminum chloride after return in stove, the gas in the second tributary directly returns in stove.
Because aluminium powder and chlorine reaction are emitted a large amount of heat, this heat is enough offset radiation dispersed heat, therefore in production process, do not need external heat, unnecessary heat carrys out balance by the shunting in the first tributary, particularly, gas in the first tributary is after overcooling collecting aluminum chloride, the tail gas forming returns in stove, the temperature of tail gas is lower than the gas temperature in the second tributary, both can balanced reaction process after mixing in heat except maintaining Reaktionsofen heat balance, can find out, can regulating stove interior reaction temperature from the ratio of air outlet expellant gas by regulating in the first tributary gas to account for.In addition, guaranteeing that under the prerequisite of reaction in furnace temperature, the gas proportion in the first tributary is larger, the rate of recovery of aluminum chloride is higher.Preferably, to account for from the volumn concentration of air outlet expellant gas be 6%～50% to the gas in the first tributary.
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 add-on the corresponding conversion aluminium powder amount of chlorine, aluminum chloride quantum of output is corresponding to be changed, but circulation gas and chlorine resultant are constant.
Fig. 1 is the schematic diagram of the device of preparing aluminum chloride of exemplary embodiment of the present.As shown in Figure 1, the device of 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 comprises body of heater, is arranged on inlet mouth on bottom of furnace body, is arranged on the air outlet on body of heater top and is arranged on the charging opening on the sidewall of body of heater middle part.Fluidization Reaktionsofen can adopt fluidization Reaktionsofen or reactor conventional in prior art, does not repeat them here.
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, the first tributary 51, cooling and collector unit 60, presser unit 40 are connected to form the first loop successively with fluidization Reaktionsofen 10, and the second tributary 52, presser unit 40 are connected to form second servo loop successively with fluidization Reaktionsofen 10.Dividing cell can adopt there is an import, two outlet T-valve, but the invention is not restricted to this, as long as dividing cell can realize shunting action.
Cooling and collector unit 60 is for cooling and collect the aluminum chloride of gas and control the temperature of reaction system.For example, when reaction in furnace system temperature is higher than 500 ℃, increase the gas flow that enters the first tributary 51, reduce the flow that gas enters the second tributary 52, after the gas in the first tributary 51 is cooling in cooling and collector unit 60 with together with gas in the second tributary 52, return in Reaktionsofen and balance stove in unnecessary heat.
Between each parts, by pipeline, connect and each pipeline on be provided with at least one valve (for example 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 be to shunting from air outlet expellant gas, otherwise, after overcooling and collector unit as the collection that is almost all liquefied of the aluminum chloride of circulation gas; When circulation gas is other gases, can shunt also and can not shunt, correspondingly operation can be by regulating the valve on each pipeline to realize.
In order to understand better above-mentioned exemplary embodiment of the present invention, below in conjunction with concrete example, it is further described.
Example 1
Outside Reaktionsofen, nitrogen is preheated to 300 ℃; After being mixed with chlorine, nitrogen after preheating passes in fluidization Reaktionsofen, the volume ratio 1:1 of nitrogen and chlorine, gas is motion from bottom to top in body of heater, when gas is full of body of heater and returns in stove by the reflux line being connected with furnace roof air outlet, stops passing into nitrogen; By the presser unit being arranged on outside fluidization Reaktionsofen, gas is pressurizeed, so that form fluidization flow field in stove; From charging opening, add aluminium powder, the mass ratio of chlorine and aluminium powder is 3.94:1, and aluminium powder also reacts and produces aluminum chloride gas with chlorine and nitrogen counter current contact in Reaktionsofen; Reacted gas is discharged rear portion gas and is entered aluminum chloride trap from the first tributary from air outlet, after its tail gas pressurization, flow back to Reaktionsofen, the remaining gas of discharging from air outlet flows back to Reaktionsofen from second direct weighting of flowing through, wherein, to account for from the volumn concentration of air outlet expellant gas be 50% to the gas in the first tributary.
Example 2
Outside Reaktionsofen, aluminum chloride gas is preheated to 500 ℃; After being mixed with chlorine, aluminum chloride gas after preheating passes in fluidization Reaktionsofen, the volume ratio 11:1 of aluminum chloride gas and chlorine, gas is motion from bottom to top in body of heater, when gas is full of body of heater and returns in stove by the reflux line being connected with furnace roof air outlet, stop passing into aluminum chloride gas; By the presser unit being arranged on outside fluidization Reaktionsofen, gas is pressurizeed, so that form fluidization flow field in stove; From charging opening, add aluminium powder, the mass ratio of chlorine and aluminium powder is 5.00:1, and aluminium powder contacts with aluminum chloride back flow of gas with chlorine and reacts and produce aluminum chloride gas in Reaktionsofen; Reacted gas is discharged rear portion gas and is entered aluminum chloride trap from the first tributary from air outlet, after its tail gas pressurization, flow back to Reaktionsofen, the remaining gas of discharging from air outlet flows back to Reaktionsofen from second direct weighting of flowing through, wherein, to account for from the volumn concentration of air outlet expellant gas be 6% to the gas in the first tributary.
Example 3
Outside Reaktionsofen, aluminum chloride gas is preheated to 400 ℃; After being mixed with chlorine, aluminum chloride gas after preheating passes in fluidization Reaktionsofen, the volume ratio 5:1 of aluminum chloride gas and chlorine, gas is motion from bottom to top in body of heater, when gas is full of body of heater and returns in stove by the reflux line being connected with furnace roof air outlet, stop passing into aluminum chloride gas; By the presser unit being arranged on outside fluidization Reaktionsofen, gas is pressurizeed, so that form fluidization flow field in stove; From charging opening, add aluminium powder, the mass ratio of chlorine and aluminium powder is 4.50:1, and aluminium powder contacts with aluminum chloride back flow of gas with chlorine and reacts and produce aluminum chloride gas in Reaktionsofen; Reacted gas is discharged rear portion gas and is entered aluminum chloride trap from the first tributary from air outlet, after its tail gas pressurization, flow back to Reaktionsofen, the remaining gas of discharging from air outlet flows back to Reaktionsofen from second direct weighting of flowing through, wherein, to account for from the volumn concentration of air outlet expellant gas be 12% to the gas in the first tributary.
Example 4
Outside Reaktionsofen, helium is preheated to 350 ℃; After being mixed with chlorine, helium after preheating passes in fluidization Reaktionsofen, the volume ratio 7:1 of helium and chlorine, gas is motion from bottom to top in body of heater, when gas is full of body of heater and returns in stove by the reflux line being connected with furnace roof air outlet, stops passing into helium; By the presser unit being arranged on outside fluidization Reaktionsofen, gas is pressurizeed, so that form fluidization flow field in stove; From charging opening, add aluminium powder, the mass ratio of chlorine and aluminium powder is 4.30:1, and aluminium powder also reacts and produces helium with chlorine and helium counter current contact in Reaktionsofen; Reacted gas is discharged rear portion gas and is entered aluminum chloride trap from the first tributary from air outlet, after its tail gas pressurization, flow back to Reaktionsofen, the remaining gas of discharging from air outlet flows back to Reaktionsofen from second direct weighting of flowing through, wherein, to account for from the volumn concentration of air outlet expellant gas be 20% to the gas in the first tributary.
Can find out, the temperature (800 ℃) of the more current Industrial Metal aluminium chlorination process of temperature of reaction (300～500 ℃) that the present invention prepares the method for aluminum chloride is low, and the liquefaction temperature of the circulation gas adopting is lower than the liquefaction temperature of aluminum chloride gas, thereby in collecting the process of 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 having described the present invention in conjunction with exemplary embodiment, it will be apparent to those skilled in the art that in the situation that do not depart from the spirit and scope that claim limits, can carry out various modifications and change to exemplary embodiment of the present invention.
Claims (7)
1. a method of preparing aluminum chloride, it is characterized in that, described method is aluminium powder to be reacted in 300～500 ℃ of fluidization flow fields with chlorine generate aluminum chloride, wherein, described 300～500 ℃ of fluidization flow fields are formed by circulation gas fluidisation, described circulation gas be not with reactive aluminum and liquefaction temperature gas and/or the aluminum chloride gas lower than the liquefaction temperature of aluminum chloride.
2. the method for preparing aluminum chloride according to claim 1, is characterized in that, said method comprising the steps of:
Warm-up cycle gas to 300～500 ℃ outside fluidization Reaktionsofen;
After being mixed with chlorine, circulation gas after preheating passes in fluidization Reaktionsofen, gas is motion from bottom to top in the body of heater of fluidization Reaktionsofen, when gas is full of body of heater and when the reflux line that is connected by the furnace roof air outlet with fluidization Reaktionsofen returns in body of heater, stops passing into circulation gas;
By the presser unit being arranged on outside fluidization Reaktionsofen, described gas is pressurizeed, so that form fluidization flow field in stove;
Add aluminium powder, aluminium powder also reacts and produces aluminum chloride gas with chlorine and circulation gas counter current contact in fluidization Reaktionsofen;
From described air outlet expellant gas through shunting after form the first tributary and the second tributary, wherein the gas in the first tributary through cooling and collect aluminum chloride after return in stove, the gas in the second tributary directly returns in stove.
3. the method for preparing aluminum chloride according to claim 2, is characterized in that, it is 6%～50% that the gas in the first tributary accounts for from the volumn concentration of air outlet expellant gas.
4. the method for preparing aluminum chloride according to claim 1, is characterized in that, described is not one or more in nitrogen, helium and argon gas with reactive aluminum and liquefaction temperature lower than the gas of the liquefaction temperature of aluminum chloride.
5. the method for 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.
6. the method for 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.
7. a device of preparing aluminum chloride, is characterized in that, described device comprises fluidization Reaktionsofen, dosage unit, air supply unit, presser unit, dividing cell and cooling and collector unit, wherein,
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 on the charging opening on the sidewall of body of heater middle part;
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, the first tributary, cooling and collector unit, presser unit are connected to form the first loop successively with fluidization Reaktionsofen, and the second tributary, presser unit are connected to form second servo loop successively with fluidization Reaktionsofen;
Cooling and collector unit is for cooling and collect the aluminum chloride of gas and control the temperature of reaction system;
Presser unit is for pressurizeing so that 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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| 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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439090A (en) * | 2015-12-14 | 2016-03-30 | 株洲冶炼集团股份有限公司 | Apparatus for preparing anhydrous metal chloride |
| CN108675332A (en) * | 2018-06-28 | 2018-10-19 | 攀钢集团钒钛资源股份有限公司 | Preparation facilities of alchlor and preparation method thereof |
| CN109942013A (en) * | 2019-05-13 | 2019-06-28 | 湖南恒光科技股份有限公司 | A kind of technique of industrial production alchlor |
| 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 |
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| 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
- 2013-09-17 CN CN201310422231.7A patent/CN103626215B/en active Active
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 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439090A (en) * | 2015-12-14 | 2016-03-30 | 株洲冶炼集团股份有限公司 | Apparatus for preparing anhydrous metal chloride |
| 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 |
| CN108675332A (en) * | 2018-06-28 | 2018-10-19 | 攀钢集团钒钛资源股份有限公司 | Preparation facilities of alchlor and preparation method thereof |
| CN109942013A (en) * | 2019-05-13 | 2019-06-28 | 湖南恒光科技股份有限公司 | A kind of technique of industrial production alchlor |
| 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 |
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| CN103626215B (en) | 2015-04-15 |
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