CN112480158A - Continuous production process of aluminum sesquiethylate chloride - Google Patents
Continuous production process of aluminum sesquiethylate chloride Download PDFInfo
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- CN112480158A CN112480158A CN202011614559.5A CN202011614559A CN112480158A CN 112480158 A CN112480158 A CN 112480158A CN 202011614559 A CN202011614559 A CN 202011614559A CN 112480158 A CN112480158 A CN 112480158A
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- Prior art keywords
- aluminum
- chloroethane
- reaction kettle
- feeding
- aluminum powder
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000010924 continuous production Methods 0.000 title claims abstract description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 46
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229960003750 ethyl chloride Drugs 0.000 claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 18
- 238000011084 recovery Methods 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 5
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 238000004064 recycling Methods 0.000 claims abstract description 5
- 239000010959 steel Substances 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims description 9
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 238000003780 insertion Methods 0.000 claims description 3
- 230000037431 insertion Effects 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 abstract description 7
- 230000007547 defect Effects 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 5
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 10
- YNLAOSYQHBDIKW-UHFFFAOYSA-M diethylaluminium chloride Chemical compound CC[Al](Cl)CC YNLAOSYQHBDIKW-UHFFFAOYSA-M 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229940100198 alkylating agent Drugs 0.000 description 1
- 239000002168 alkylating agent Substances 0.000 description 1
- 238000012648 alternating copolymerization Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 150000001399 aluminium compounds Chemical class 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- 229940077746 antacid containing aluminium compound Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- UAIZDWNSWGTKFZ-UHFFFAOYSA-L ethylaluminum(2+);dichloride Chemical compound CC[Al](Cl)Cl UAIZDWNSWGTKFZ-UHFFFAOYSA-L 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000002685 polymerization catalyst Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/06—Aluminium compounds
- C07F5/061—Aluminium compounds with C-aluminium linkage
- C07F5/064—Aluminium compounds with C-aluminium linkage compounds with an Al-Halogen linkage
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a continuous production process of aluminum sesquiethyl chloride, which comprises the steps of adding a certain amount of aluminum sesquiethyl into a reaction kettle from a chloroethane feeding steel cylinder, wherein the liquid level is just right to a filter port of the reaction kettle; respectively metering chloroethane and aluminum powder by using inert gas delivery, controlling the chloroethane feeding speed through a first valve, controlling the aluminum powder feeding speed in an aluminum powder metering tank through a second valve, and slowly feeding the aluminum powder into a reaction kettle for continuous reaction; and controlling a third valve to maintain the pressure of the reaction kettle, transferring the materials in the chloroethane recovery tank into a chloroethane metering tank for recycling, and realizing continuous production through quantitative feeding and discharging. The invention solves the problems that the methods for synthesizing the sesquiethyl aluminum are all high-pressure batch methods, the batch method has the defects of more equipment, low conversion rate, more waste residues, more dangerous points and the like in production, continuous production cannot be realized, the investment is increased in large-scale production, the energy consumption is increased, and the risk is increased.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a continuous production process of aluminum sesquiethylate chloride.
Background
The aluminum sesquiethyl, also known as aluminum sesquiethyl chloride, is a colorless liquid with CAS number 12075-68-2. The sesquiethylaluminum chloride is a chemical substance, is an intermediate for preparing organic aluminium compounds of triethyl aluminium, diethyl aluminium chloride, dichloroethylaluminum, etc., and can also be used for preparing olefin polymerization catalyst, butadiene and methyl methacrylateA cool alternating copolymerization catalyst. The sesquiethyl aluminum chloride has active chemical property, can be used as a catalyst, an alkylating agent, a reducing agent, an intermediate for preparing organic compounds and the like in the polyolefin industry, and has very wide application. There are three current methods for synthesizing aluminum sesquiethylate chloride: 1. by direct reaction of metallic aluminium with ethyl chloride to form sesqui-3 (C)2H5) Cl+2Al→(C2H5)3Al2Cl3(ii) a 2. The pure diethyl aluminum monochloride is directly obtained by reacting aluminum magnesium alloy with ethyl chloride. Then reacting with aluminum trichloride to obtain aluminum sesquiethyl, Al2Mg+4C2H5Cl→2(C2H5)2AlCl+MgCl2，3(C2H5)2AlCl+2AlCl3→3(C2H5)3Al2Cl3(ii) a 3. Synthesizing triethyl aluminum directly by using aluminum, hydrogen and ethylene under high pressure, and then reacting with aluminum trichloride to obtain sesquiethyl aluminum, 3 (C)2H4) +Al+3/2 H2→(C2H5)3Al，(C2H5)3Al+AlCl3→(C2H5)3Al2Cl3。
At present, the method for synthesizing the sesquiethyl aluminum is a high-pressure batch method, the batch method has the defects of more equipment, low conversion rate, more waste residues, more dangerous points and the like in production, continuous production cannot be realized, and the problems of increased investment, increased energy consumption, increased risk and the like are caused in large-scale production, so that a continuous production process of the sesquiethyl aluminum chloride is designed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a continuous production process of aluminum sesquiethylate, which solves the problems that the methods for synthesizing the aluminum sesquiethylate are all high-pressure batch methods, the batch method production has the defects of more equipment, low conversion rate, more waste residues and more dangerous points, the continuous production cannot be realized, the investment is increased during large-scale production, the energy consumption is increased, and the risk is increased.
In order to achieve the purpose, the invention adopts the technical scheme that:
a continuous production process of aluminum sesquiethyl chloride comprises the following steps,
(1) adding a certain amount of aluminum sesquiethyl into the reaction kettle from a chloroethane feeding steel cylinder, wherein the liquid level is just to the filter port of the reaction kettle;
(2) respectively metering chloroethane and aluminum powder by using inert gas delivery, controlling the chloroethane feeding speed through a first valve, controlling the aluminum powder feeding speed in an aluminum powder metering tank through a second valve, and slowly feeding the aluminum powder into a reaction kettle for continuous reaction;
(3) controlling a third valve to maintain the pressure of the reaction kettle, and slowly transferring the material into a flash evaporator by controlling the total flow rate of discharged materials through an inserting pipe (13) with a filter screen arranged in the reaction kettle and a second flow meter;
(4) the materials enter a flash evaporator for flash separation;
(5) collecting the first component product collected by the first-stage condenser at 10-30 ℃ into a product tank through second-stage condensation separation, and collecting the fraction collected by the second-stage condenser at-10-10 ℃ into a chloroethane recovery tank;
(6) transferring the materials in the chloroethane recovery tank into a chloroethane metering tank for recycling, and realizing continuous production through quantitative feeding and discharging.
In the continuous production process of the sesquiethyl aluminum chloride, in the step (1), the filter opening is a filter plate or a filter screen structure, the aperture R is 200-500 meshes, and the reaction kettle is stirred at the temperature of 45-85 ℃.
In the aforementioned continuous production process of aluminum sesquiethyl chloride, in the step (2), the mesh number of the aluminum powder is 150-450 meshes, the feeding speed of ethyl chloride is as follows: and continuously feeding aluminum powder at a feeding speed of 2.8:1-3.3:1 according to a mass ratio of 3.6:1-4.2: 1.
In the continuous production process of the aluminum sesquiethylate, in the step (3), the pressure of the reaction kettle is 0.4-0.7 MPa.
In the continuous production process of the aluminum sesquiethylate, in the step (4), the flash evaporator 6 is operated at a temperature of 100 ℃ and a pressure of 130 ℃: flash separation is carried out under the condition of-0.06-0.09 MPa.
The invention has the beneficial effects that: according to the invention, chloroethane and aluminum powder are respectively added into a reaction kettle for reaction, reaction liquid in the reaction kettle is slowly fed into a flash evaporator through a feeding pump for distillation, after the distillation is finished, a first component product collected by a first-stage condenser at 10-30 ℃ is collected into a product tank, a second component product collected by a second-stage condenser at-10-10 ℃ is collected into a chloroethane recovery tank, the collected stable temperature is most suitable for chloroethane, the recovery efficiency is high, and the residue is less. The method solves the problems that the methods for synthesizing the sesquiethyl aluminum are all high-pressure batch methods, the batch method has the defects of more equipment, low conversion rate, more waste residues, more dangerous points and the like, continuous production cannot be realized, investment is increased during large-scale production, energy consumption is increased, and risk is increased.
Drawings
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a flow chart of the production apparatus of the present invention.
In the figure: 1. the device comprises a reaction kettle, 2 parts of a first valve, 3 parts of a second valve, 4 parts of an aluminum powder metering tank, 5 parts of a third valve, 6 parts of a flash evaporator, 7 parts of a primary condenser, 8 parts of a secondary condenser, 9 parts of a chloroethane recovery tank, 10 parts of a chloroethane feeding steel cylinder, 11 parts of a first flowmeter, 12 parts of a second flowmeter, 13 parts of an insertion pipe.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to FIGS. 1-2: a continuous production process of aluminum sesquiethyl chloride comprises the following steps,
(1) adding a certain amount of sesquiethyl aluminum into the reaction kettle 1 from a chloroethane feeding steel bottle 10, wherein the liquid level is just right to the filter port of the reaction kettle 1;
(2) respectively metering chloroethane and aluminum powder by using inert gas conveying, controlling the chloroethane feeding speed through a first valve 2, controlling the aluminum powder feeding speed in an aluminum powder metering tank 4 through a second valve 3, and slowly adding the chloroethane and the aluminum powder into a reaction kettle 1 for continuous reaction;
(3) controlling a third valve 5 to maintain the pressure of the reaction kettle 1, and slowly transferring the material into a flash evaporator 6 by controlling the total flow rate of the discharged material through an insertion pipe 13 with a filter screen arranged in the reaction kettle 1 and a second flow meter 12;
(4) the materials enter a flash evaporator 6 for flash separation;
(5) collecting the first component product collected by the first-stage condenser 7 at 10-30 ℃ into a product tank through second-stage condensation separation, and collecting the fraction collected by the second-stage condenser 8 at-10-10 ℃ into a chloroethane recovery tank 9;
(6) and materials in the chloroethane recovery tank 9 are transferred into a chloroethane metering tank for recycling, and continuous production is realized through quantitative feeding and discharging.
Preferably, in the step (1), the filter port is a filter plate or a filter screen structure, the aperture R is 200-500 meshes, and the reaction kettle is stirred at the temperature of 45-85 ℃.
Preferably, in the step (2), the mesh number of the aluminum powder is 150-450 meshes, and the feeding speed of the chloroethane is as follows: and continuously feeding aluminum powder at a feeding speed of 3.6:1-4.2:1 by mass ratio.
Preferably, in the step (3), the pressure of the reaction kettle 1 is 0.4-0.7 MPa.
Preferably, in the step (4), the flash evaporator (6) is operated at a temperature of 100 ℃ and a temperature of 130 ℃, and the pressure: flash separation is carried out under the condition of-0.06-0.09 MPa.
Example 1, (A1) 500kg of aluminum sesquiethyl was charged into a 2000L reactor 1, the liquid level was at the filter port of the reactor 1, the filter port was a 200 mesh filter plate, the reactor 1 was started to stir, and preheating was carried out at a temperature of 65 ℃;
(A2) conveying by using inert gas nitrogen, controlling by a first flow meter 11 and a second valve 3, adding 150 meshes of aluminum powder into a reaction kettle 1 at a feeding speed of 0.44Kg/min, simultaneously adding ethyl chloride into the reaction kettle 1 at a feeding speed of 1.76Kg/min, and slowly reacting while the pressure of the reaction kettle 1 is slowly increased, wherein the pressure is maintained between 0.4 and 0.7 MPa;
(A3) preheating the flash evaporator 6 to 120 ℃ in advance, and maintaining the pressure at-0.08 MPa by using a vacuum pump;
(A4) the pressure of the reaction kettle 1 is utilized, the material is controlled by a second flowmeter 12 and a third valve 5, the material passes through a filter plate, and the material is slowly transferred into a flash evaporator 6 for flash evaporation at the discharging speed of 2.2 Kg/min;
(A5) the material is separated by secondary condensation, the first component product collected by the primary condenser 7 at 15 ℃ is collected into a product tank, the collection speed is 2.0Kg/min, the fraction collected by the secondary condenser 8 at-9 ℃ is collected into a chloroethane recovery tank 9, and the collection speed is 0.2 Kg/min;
(A6) materials in the chloroethane recovery tank 9 are transferred into a chloroethane metering tank for recycling, and continuous production is realized through quantitative feeding of 2.2Kg/min and discharging of 2.2 Kg/min.
In conclusion, when the device is used, the chloroethane and the aluminum powder are respectively added into the reaction kettle for reaction, the reaction liquid in the reaction kettle is slowly fed into the flash evaporator through the feeding pump for distillation, and after the distillation is finished, the product is collected. The method solves the problems that the methods for synthesizing the sesquiethyl aluminum are all high-pressure batch methods, the batch method has the defects of more equipment, low conversion rate, more waste residues, more dangerous points and the like, continuous production cannot be realized, investment is increased during large-scale production, energy consumption is increased, and risk is increased.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (5)
1. A continuous production process of aluminum sesquiethyl chloride is characterized in that: comprises the following steps of (a) carrying out,
(1) adding a certain amount of sesquiethyl aluminum into the reaction kettle (1) from a chloroethane feeding steel cylinder (10), wherein the liquid level is just right to the filter port of the reaction kettle (1);
(2) conveying by using inert gas, respectively metering chloroethane and aluminum powder, controlling the chloroethane feeding speed through a first valve (2), controlling the aluminum powder feeding speed in an aluminum powder metering tank (4) through a second valve (3), and slowly feeding the chloroethane and the aluminum powder into a reaction kettle (1) for continuous reaction;
(3) controlling a third valve (5) to maintain the pressure of the reaction kettle (1), and slowly transferring the material into a flash evaporator (6) by controlling the total flow rate of the discharged material through an insertion pipe (13) with a filter screen arranged in the reaction kettle (1) and a second flow meter (12);
(4) the materials enter a flash evaporator (6) for flash separation;
(5) collecting the first component product collected by the first-stage condenser (7) at 10-30 ℃ into a product tank through secondary condensation separation, and collecting the fraction collected by the second-stage condenser (8) at-10-10 ℃ into a chloroethane recovery tank (9);
(6) materials in the chloroethane recovery tank (9) are transferred into a chloroethane metering tank for recycling, and continuous production is realized through quantitative feeding and discharging.
2. A continuous process for the production of aluminum sesquiethylate chloride according to claim 1, characterized in that: in the step (1), the filter opening is a filter plate or a filter screen structure, the aperture R is 200-500 meshes, and the reaction kettle is stirred at the temperature of 45-85 ℃.
3. A continuous process for the production of aluminum sesquiethylate chloride according to claim 1, characterized in that: in the step (2), the mesh number of the aluminum powder is R-50, namely 150-450 meshes, and the feeding speed of the chloroethane is as follows: and continuously feeding aluminum powder at a feeding speed of 3.6:1-4.2:1 by mass ratio.
4. A continuous process for the production of aluminum sesquiethylate chloride according to claim 1, characterized in that: in the step (3), the pressure of the reaction kettle (1) is 0.4-0.7 MPa.
5. A continuous process for the production of aluminum sesquiethylate chloride according to claim 1, characterized in that: in the step (4), the flash evaporator (6) is operated at a temperature of 100 ℃ and a pressure of 130 ℃: flash separation is carried out under the condition of-0.06-0.09 MPa.
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| CN202011614559.5A CN112480158A (en) | 2020-12-31 | 2020-12-31 | Continuous production process of aluminum sesquiethylate chloride |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011614559.5A CN112480158A (en) | 2020-12-31 | 2020-12-31 | Continuous production process of aluminum sesquiethylate chloride |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB830884A (en) * | 1958-10-24 | 1960-03-23 | Huels Chemische Werke Ag | Improvements in the production of alkylaluminium sesquichlorides |
| CN106866718A (en) * | 2017-02-10 | 2017-06-20 | 安徽博泰电子材料有限公司 | A kind of preparation method of sesquialter aikyl aluminum halide |
| CN108358962A (en) * | 2018-04-13 | 2018-08-03 | 山东亿盛实业股份有限公司 | A kind of method for continuously synthesizing of methyl sesquialter aluminium |
-
2020
- 2020-12-31 CN CN202011614559.5A patent/CN112480158A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB830884A (en) * | 1958-10-24 | 1960-03-23 | Huels Chemische Werke Ag | Improvements in the production of alkylaluminium sesquichlorides |
| CN106866718A (en) * | 2017-02-10 | 2017-06-20 | 安徽博泰电子材料有限公司 | A kind of preparation method of sesquialter aikyl aluminum halide |
| CN108358962A (en) * | 2018-04-13 | 2018-08-03 | 山东亿盛实业股份有限公司 | A kind of method for continuously synthesizing of methyl sesquialter aluminium |
Non-Patent Citations (1)
| Title |
|---|
| 袁履冰 等编著, 人民教育出版社 * |
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