CN107661734B - Solid-liquid phase reaction apparatus and method for producing metal alkoxide compound - Google Patents
Solid-liquid phase reaction apparatus and method for producing metal alkoxide compound Download PDFInfo
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- CN107661734B CN107661734B CN201610616535.0A CN201610616535A CN107661734B CN 107661734 B CN107661734 B CN 107661734B CN 201610616535 A CN201610616535 A CN 201610616535A CN 107661734 B CN107661734 B CN 107661734B
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/085—Feeding reactive fluids
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- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
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- C07C29/70—Preparation of metal alcoholates by converting hydroxy groups to O-metal groups
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Abstract
The invention relates to the technical field of solid-liquid phase reaction, and discloses a solid-liquid phase reaction device and a method for preparing a metal alkoxide compound. The device comprises a closed reactor shell (1) and a component which is arranged in the closed reactor shell and used for limiting a reaction area, wherein the upper part of the closed reactor shell is provided with a solid inlet (6) and a gas phase material outlet (8), and the bottom and/or the side wall of the closed reactor shell is provided with a liquid inlet. The solid-liquid phase reaction device provided by the invention can realize sufficient contact and reaction of solid-liquid two phases, and can use solid reactants with larger particle size (such as block shape) as reaction raw materials.
Description
Technical Field
The invention relates to the technical field of solid-liquid phase reaction, in particular to a solid-liquid phase reaction device and a method for preparing a metal alkoxide compound by adopting the solid-liquid phase reaction device.
Background
The reaction in which the liquid and solid are brought into contact with each other is one of the most common reactions in engineering, most typically the reaction between a metal or a mixture of metals and a fatty alcohol or a mixture of fatty alcohols. The characteristics of this type of reaction are: the reaction is strongly exothermic, a large amount of hydrogen is generated in the reaction process, and the product generated in the reaction is simultaneously the catalyst of the reaction, namely, the autocatalytic reaction, so that if the reaction process is not controlled, the reaction speed can be rapidly increased, a large amount of heat and hydrogen are generated, and the explosion risk is caused. Therefore, in the reaction process, the design difficulty of the reactor is that how to fully contact and react the solid and the liquid which participate in the reaction, how to realize the continuous addition of the raw materials and the continuous extraction of the product, and simultaneously, the generated product can be uniformly distributed in the reaction system and is easy to be separated from the solid material which participates in the reaction. Another design difficulty of the solid-liquid phase reactor is how to control the controllable reaction of the strong heat release and autocatalysis, and the reaction can be rapidly stopped when the reaction is too violent and difficult to control, so that the operation accident is avoided, and the safe and stable operation of the production process is ensured.
US4590289 discloses an apparatus and process for the continuous production of aluminium alkoxide by reaction of a C3-C10 alcohol with aluminium metal, the apparatus comprising a reactor with a housing, the aluminium metal being fed from the top of the reactor and reacted with an aluminium alkoxide/alcohol mixture, the aluminium alkoxide and alcohol mixture being on a plate with openings or a tray with a screen. The reaction area is formed by the area, the liquid storage tank is arranged at the lower part of the reaction area, the liquid after reaction falls into the area from the side wall perforated plate at the periphery of the reaction area, a part of the liquid is sent out as a product, and most of the liquid is mixed with condensed and refluxed alcohol and returns to the reaction area. One part of the liquid phase mixture returned to the reaction area enters the reactor after being mixed with the metallic aluminum from the upper part of the reactor, and the other part enters the reaction area from the lower part of the slot plate. Meanwhile, in order to ensure that the metal aluminum particles can be fully mixed and contacted with the liquid, the metal aluminum particles are needle-shaped, the diameter is 0.5-0.8mm, and the length is 5-12 mm. The technical scheme of the patent application realizes the continuous feeding of the metal aluminum and the fatty alcohol, and can quickly stop the reaction when the reaction is out of control, but the reaction has the defects that the backflow of a large amount of liquid-phase materials causes extremely high energy consumption, and meanwhile, the manufacturing process of the fine metal aluminum particles is complex and expensive, so that the production cost is greatly increased; in addition, metal aluminum particles are too small, a metal net can be blocked in a long-term reaction process, and a solid phase and a liquid phase cannot be rapidly separated when the reaction is out of control after the screen is blocked, so that the danger in the reaction process is increased.
US6428757B1 proposes an improved solid-liquid phase reactor aiming at the disadvantages of the above reactor, which improves the fixed perforated plate/screen of the reaction area into a rotatable grid, which makes the reacted solid easily and uniformly distributed in the reaction area and more fully contacted with the liquid, and also makes it possible to use larger metallic aluminum blocks for reaction, but the design of the device is more complicated, the rotating reaction area also increases the larger energy consumption, and the device has great operation difficulty and high maintenance cost.
US6017499 proposes a drum reactor comprising a perforated screen drum. The screen is a rotary drum screen, the drum screen is arranged on at least one hollow shaft, the at least one hollow shaft is provided with a device for conveying solids, and the conveyed solids enter the interior of the drum screen through the hollow shaft; during operation the trommel is rotated in a bottom tank which contains a liquid medium which reacts with the solids. The sump can be lowered, i.e. the solids in the drum and the liquid in the sump can be separated from each other if necessary, and the reaction can be changed or interrupted as desired. When using a solid trommel, it is no longer necessary to circulate a large amount of reaction liquid. The drum screen enables the solid to continuously move in the reaction area, so that the solid and the liquid are fully contacted with each other, and the suspension state of the solid does not need to be maintained through the circulation of the liquid. Because the bottom tank can descend, the liquid in the bottom tank and the solid in the drum screen can be separated to different degrees, and therefore the reaction is effectively controlled. The reactor realizes the continuous addition of the metal aluminum and the fatty alcohol, and simultaneously can realize the solid-liquid two-phase separation through the descending of the liquid storage tank so as to ensure that the reaction is in a controllable range, but the reactor also has a plurality of problems, and because the reaction is carried out in the roller and a central shaft for conveying solids is arranged in the roller, the actual reaction interval is very small; in addition, the solid is conveyed through the central shaft, so that the shape and the size of the solid are strictly required; the separation of solid and liquid is actually realized by a rope winch for lowering a liquid storage tank at the bottom, so that the difficulty of actual operation and maintenance is increased. The whole reactor has relatively complex structure and difficult maintenance.
US2010/0152471 proposes a solid-liquid or gas-solid phase reactor comprising a closed vessel partially filled with a liquid, a metal basket in the vessel, the solid being contained in the metal basket, the metal basket being oscillated relative to the vessel, the solid being contacted with the liquid in the basket. Liquid is sprayed into the vessel from the upper part of the reactor through a plurality of spray ports, and solid is added into a reaction area in a metal basket in the vessel through two distributors. The structural design of the reactor is relatively simple compared with the drum reactor proposed in US6017499, but since the metal basket oscillates back and forth relative to the reactor, when aluminum metal is added into the reactor, the oscillation of the metal basket inside the reactor needs to be stopped temporarily, which increases the complexity of the operation of the apparatus, increases the energy consumption, and simultaneously reduces the service life of the oscillating motor.
Disclosure of Invention
The invention aims to provide a solid-liquid phase reaction device which has simple design, can continuously and fully contact a solid phase and a liquid phase for reaction and has low operation and maintenance cost and a method for preparing a metal alkoxide compound.
The invention provides a solid-liquid phase reaction device which comprises a closed reactor shell and a component which is arranged in the closed reactor shell and used for limiting a reaction area, wherein a solid inlet and a gas phase material outlet are arranged at the upper part of the closed reactor shell, and a liquid inlet is arranged at the bottom and/or the side wall of the reactor shell.
In one embodiment, the means for delimiting the reaction zone is a metal partition with an opening, which divides the interior of the closed reactor shell into an upper and a lower part. In this embodiment, the metal partition is provided with a plurality of liquid inlets, the liquid inlets are disposed at the bottom of the closed reactor shell, and the solid inlet and the gas-phase material discharge outlet are disposed at the top of the closed reactor shell.
In another embodiment, the means for delimiting the reaction zone is a fixing kit provided with openings in the upper opening, sides and bottom, which divides the interior of the closed reactor shell into an inner and an outer part. In this embodiment, the liquid inlet is provided at one or more of the top, bottom and sides of the closed reactor shell, the solids inlet is provided at the top of the closed reactor shell, and the bottom and/or sides of the closed reactor shell are provided with a stirring gas inlet.
The present invention also provides a process for producing a metal alkoxide compound using the above solid-liquid phase reaction apparatus, wherein a fatty alcohol is fed through the liquid inlet, and a metal reactant is fed through the solid inlet, and the fatty alcohol and the metal reactant are subjected to a contact reaction in the reaction zone.
In the solid-liquid phase reaction device provided by the invention, a boiling liquid layer can be formed in the reaction area in the closed reactor shell due to the entering of a liquid phase reactant or the introduction of stirring gas and the rising of reaction generated gas, so that the solid-liquid two-phase full contact and reaction can be realized, and the solid reactant with larger particle size (such as block shape) can be used as a reaction raw material, thereby solving the problems that the existing solid-liquid phase reaction device cannot adopt larger block-shaped solid phase reactant, and the equipment structure is complicated due to the adoption of the rotation or the swing of a screen in the reactor to realize the solid-liquid two-phase full contact. Moreover, the solid-liquid phase reaction device has low manufacturing cost, easy operation and low operation and equipment maintenance cost.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic configuration diagram of a solid-liquid phase reaction apparatus according to a first embodiment of the present invention;
fig. 2 is a schematic structural view of a solid-liquid phase reaction apparatus according to a second embodiment of the present invention.
Description of the reference numerals
1 closed reactor shell 2a Metal baffle
2b fixing the sleeve 3 open
4 fixed external member support 5 metal baffle fixed component
6 solid inlet 7a upper valve
7b lower valve 8 gas phase material outlet
9,10 condenser 11 flow meter
12,13 emergency storage tank 14 inert gas purge line
15 inert gas exhaust line 16 liquid reactant inlet line
17 liquid phase material inlet and circulating pipeline 18 product discharge pipeline
19,20 product take-off and recycle line 21 product withdrawal line
22,23 emergency discharge lines 24a,24b condensate return line
25 gas material discharge line
27 gas discharge line 28,29 stirring gas line
31 gas compressor
A, B, C, D, E, F: liquid inlet on metal separator in fig. 1
H, I, J, K, L: liquid inlet on the closed reactor shell in fig. 2
a, b, c, d: stirring gas inlet on the closed reactor shell in FIG. 2
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
As shown in fig. 1 and 2, the present invention provides the solid-liquid phase reaction apparatus comprising: a closed reactor shell 1 and components arranged in the closed reactor shell for defining a reaction area, wherein the upper part of the closed reactor shell is provided with a solid inlet 6 and a gas phase material outlet 8, and the bottom and/or the side wall of the closed reactor shell is provided with a liquid inlet.
In the solid-liquid phase reaction device provided by the invention, the components for defining the reaction area are arranged, and a solid inlet is arranged at the upper part of the closed type reactor shell 1, a liquid inlet is arranged at the bottom and/or the side wall of the closed type reactor shell, and preferably a stirring gas inlet is arranged, so that the solid-liquid phase reaction device can form a boiling liquid layer in the reaction area due to the entering of liquid phase reaction materials, the introduction of stirring gas and the rising of gas generated by reaction when in use, and the solid reactant and the liquid reactant can be in contact reaction in the boiling liquid layer. The specific arrangement of the means for defining the reaction region is not particularly limited in the present invention.
According to the first embodiment of the present invention, as shown in fig. 1, in the solid-liquid phase reaction apparatus, the means for defining the reaction region is a metal partition plate 2a having an opening 3, and the metal partition plate 2a divides the interior of the closed reactor shell 1 into upper and lower portions. In this embodiment, it is preferable that the metal partition plate 2a is provided with a plurality of liquid inlets, a pipeline connected to the liquid inlets passes through the bottom of the closed reactor shell 1 (i.e., the liquid inlets on the metal partition plate 2a are connected to the liquid inlets on the bottom of the closed reactor shell 1 through pipelines), and the solid inlet and the gas-phase material discharge port are provided at the top of the closed reactor shell 1.
According to the solid-liquid phase reaction apparatus of the above embodiment, in the internal space of the closed reactor shell 1, the upper portion of the metal partition plate 2a is defined as a reaction region. The liquid reactant is injected into the reaction zone through a liquid inlet at the bottom of the closed reactor shell 1 and via a plurality of liquid inlets on the metal separator 2a, forming a liquid layer in the reaction zone; solid reactant is fed into the reaction zone through a solid inlet at the top of the closed reactor shell 1, and the solid reactant and liquid reactant react in the liquid layer to boil the liquid layer. The mixture of the reaction product and the liquid reactant (i.e., the liquid-phase material) flows out from the opening of the metal separator 2a into the lower region of the metal separator 2a (i.e., the lower half portion of the internal space of the closed-type reactor shell 1), and is then pumped out. The pumped liquid phase material can be sprayed into the liquid inlet at the bottom of the closed reactor shell 1 and returned to the reaction area through the liquid inlet on the metal partition plate 2a, so as to maintain the height of the liquid layer in the reaction area, and the other part can be pumped out as a product.
In the solid-liquid phase reaction apparatus of the above embodiment, the metal partition plate 2a divides the internal space of the closed reactor shell 1 into upper and lower portions, and the volume ratio of the upper and lower portions may be 1/1 to 9/1, preferably 3/1 to 5/1.
In the solid-liquid phase reactor of the above embodiment, the openings of the metal partition plate 2a allow the gas-phase material and the liquid-phase material to pass therethrough, while the solid-phase material cannot pass therethrough and is trapped at the upper portion of the metal partition plate 2 a. Preferably, the average diameter of the openings is 0.5 to 50mm, more preferably 0.5 to 20 mm. The opening ratio of the metal separator 2a may be 30 to 95%, preferably 60 to 90%. The shape of the opening is not particularly limited, and may be, for example, circular, elliptical, polygonal, or amorphous, and preferably circular or quadrangular.
In the solid-liquid phase reaction apparatus of the above embodiment, the solid-liquid phase reaction apparatus may further include a condenser communicating with the gas-phase feed outlet provided at the top of the closed reactor shell 1. And gas materials generated by the reaction in the closed reactor shell 1 are discharged through a gas-phase material outlet and enter the condenser for condensation. Preferably, condensate condensed from the condenser flows back into the closed reactor shell 1 through the liquid inlet.
In the solid-liquid phase reaction apparatus of the above embodiment, the metal partition plate 2a may be installed or fixed in the closed reactor shell 1 in a conventional manner, for example, the metal partition plate 2a is fixed in the closed reactor shell 1 by a metal partition plate fixing assembly 5, the fixing assembly 5 is installed in such a manner that the inner space of the closed reactor shell 1 is divided into an upper portion and a lower portion by the metal partition plate 2a, and the upper portion and the lower portion are communicated only through the opening of the metal partition plate 2 a.
According to a second embodiment of the present invention, as shown in fig. 2, in the solid-liquid phase reaction apparatus, the means for defining the reaction region is a fixing kit 2b having an opening at the upper part, the side part and the bottom part, and the fixing kit 2b divides the inside of the closed reactor shell 1 into an inner part and an outer part. In this embodiment, preferably, the liquid inlet is provided at one or more of the top, bottom and side portions of the closed reactor shell 1, the solid inlet and the gas-phase material discharge port are provided at the top portion of the closed reactor shell 1, and the bottom and/or side portion of the closed reactor shell 1 is provided with an agitating gas inlet.
According to the solid-liquid phase reaction apparatus of the above embodiment, in the internal space of the closed reactor shell 1, the inside of the fixing kit 2b is defined as a reaction area. Liquid reactants are injected into the reaction zone through liquid inlets at one or more of the top, bottom and sides of the closed reactor shell 1 via the openings 3 in the fixed sleeve 2b and stirring gas is injected through stirring gas inlets at the bottom and/or sides of the closed reactor shell 1, forming a boiling liquid layer in the reaction zone; solid reactant is fed into the reaction zone through a solid inlet 6 at the top of the closed reactor shell 1 and the solid reactant and liquid reactant react in the boiling liquid layer. The mixture of reaction products and liquid reactants, i.e. the liquid phase material, flows out of the openings in the fixed sleeve 2b, enters the outer region of the fixed sleeve 2b and is subsequently pumped out at the bottom of the closed reactor shell 1. Part of the liquid phase material pumped out can be circularly sprayed into the closed type reactor shell 1 through the liquid inlet, and the other part can be pumped out as a product.
When a liquid reactant is injected from the top of the closed reactor shell 1, the liquid reactant directly enters the reaction area (i.e., inside the fixing kit 2b) and directly contacts with a solid reactant to react. When liquid reactant is injected from the side and the bottom of the closed type reactor shell 1, the fixing sleeve 2b can be washed, and the opening on the fixing sleeve 2b is kept smooth.
In the above embodiment, the stirring gas inlet provided at the bottom and/or the side of the closed reactor shell 1 is used for stirring the materials in the reaction region, increasing the contact between the solid-liquid phase reactants, accelerating the reaction, and simultaneously dispersing the reaction products in the liquid phase materials rapidly and uniformly. The stirring mode avoids the defects of difficult addition of solid reactants, complex operation and high energy consumption generated when the internal sleeve of the reactor swings or the whole reactor rotates, is easier to implement, and has lower equipment operation and maintenance cost.
In the solid-liquid phase reaction apparatus of the above embodiment, the fixing kit 2b divides the inside of the closed reactor shell 1 into an inner part and an outer part, and the volume ratio of the inner part to the outer part may be 9/1 to 1/3, preferably 5/1 to 1/1.
In the solid-liquid phase reaction apparatus of the above embodiment, the openings of the fixing member 2b allow the gas-phase material and the liquid-phase material to pass therethrough, but the solid-phase material cannot pass therethrough and is trapped in the inner region of the fixing member 2 b. Preferably, the average diameter of the openings is 0.1 to 50mm, more preferably 0.5 to 20 mm. The aperture ratio of the fixing kit 2b may be 30-95%, preferably 60-90%. The shape of the opening is not particularly limited, and may be, for example, circular, elliptical, polygonal, or amorphous, and preferably circular or quadrangular.
In the solid-liquid phase reaction apparatus of the above embodiment, the fixing kit 2b may be installed or fixed in the closed reactor shell 1 in a conventional manner, for example, the fixing kit 2b is fixed in the closed reactor shell 1 by a fixing kit bracket 4, the bracket 4 is installed in such a manner that the inner space of the closed reactor shell 1 is divided into an inner part and an outer part by the fixing kit 2b, and the outer space of the fixing kit 2b is communicated.
In the solid-liquid phase reaction apparatus of the above embodiment, the solid-liquid phase reaction apparatus may further include a condenser communicating with a gas-phase feed discharge port provided at the top of the closed reactor shell 1. And gas materials generated by the reaction in the closed reactor shell 1 are discharged through a gas-phase material discharge port and enter the condenser for condensation. Preferably, condensate condensed from the condenser flows back into the closed reactor shell 1 through the liquid inlet; the non-condensable gas may be recycled into the stirring gas inlet at the side and/or bottom of the closed reactor shell 1 for use as a stirring gas to further reduce the production cost.
In the present invention, the condenser may be a condenser conventional in the art, and may be, for example, an air-cooled condenser or a water-cooled condenser, preferably a water-cooled condenser. The water-cooled condenser can be in a vertical type, a horizontal type, an evaporation type and the like, and is preferably in a vertical type or a horizontal type.
In the present invention, the solid-liquid phase reaction apparatus may further include one or more emergency storage tanks, which are communicated with the bottom of the closed reactor shell 1. When the reaction is too violent and out of control, the circulation of the liquid phase material can be stopped immediately, and simultaneously the liquid phase material in the closed reactor shell 1 is discharged into an emergency storage tank rapidly, so that the reaction is stopped. In order to achieve a complete separation of the solid-liquid phases in an emergency, the volume of the emergency storage tank or the sum of the volumes of the multiple storage tanks is not less than the volume of the closed reactor shell 1.
In the invention, preferably, a solid feeding hopper is arranged on the solid inlet 6 of the device, an upper valve 7a and a lower valve 7b are arranged at the lower part of the hopper, a space is reserved between the two valves, and an inert gas purging port is arranged on the side wall of the space. The container between the two valves may be a cylinder, an elliptical cylinder, a rectangular cylinder, a cubic cylinder or a polygonal cylinder, preferably a cylinder or a cubic cylinder. The inert gas purged by the inert gas purging port may be nitrogen, carbon dioxide or a rare gas (helium, neon, argon, krypton, xenon, radon), preferably nitrogen or carbon dioxide. Specifically, the manner of adding the solid reactant through the solid inlet includes: firstly, solid reactant enters a container between the valves through the upper valve 7a, the upper valve 7a and the lower valve 7b are closed, inert gas is introduced to replace oxygen carried by the solid reactant, then the lower valve 7b is opened, the upper valve is kept closed, and the solid enters a reaction area through the lower valve 7 b. The solid inlet may be one, two or more, preferably one or two depending on the size of the reactor.
In the solid-liquid phase reactor provided by the invention, part of the liquid material discharged from the closed reactor shell 1 is recycled back to the closed reactor shell 1 through the liquid inlet, and part of the liquid material is extracted as a product.
In the present invention, the closed reactor shell 1 may be in various conventional shapes, for example, a cube, a rectangular parallelepiped, a cylinder, an elliptical cylinder, a sphere, etc., preferably a cylinder, an elliptical cylinder or a rectangular parallelepiped.
The solid-liquid phase reaction device provided by the invention can use a solid reactant with a larger size as a reaction raw material, and the particle size of the solid reactant can be 0.1-80cm, and is preferably 3-20 cm.
The present invention also provides a process for producing a metal alkoxide compound using the above solid-liquid phase reaction apparatus, wherein a fatty alcohol is fed through the liquid inlet, and a metal reactant is fed through the solid inlet, and the fatty alcohol and the metal reactant are subjected to a contact reaction in the reaction zone.
In the present invention, the fatty alcohol may be C1To C12In an alcohol of (1)At least one, preferably at least one of the alcohols C3 to C8, such as one or more of n-butanol, n-pentanol and n-hexanol.
In the present invention, the metal reactant may be at least one of magnesium, aluminum, zinc and zirconium, preferably aluminum and/or magnesium. The particle size of the metal reactant may be in the range of 0.1 to 80cm, preferably 3 to 20 cm.
In the present invention, the liquid layer height of the reaction zone within the closed reactor shell 1 may be 1.2 to 5 times, preferably 1.5 to 3 times, the average particle size of the metal reactant.
In the present invention, a part of the liquid-phase material discharged from the closed reactor shell is recycled to the reactor, and the mass ratio of the recycled material to the discharged material may be 1/1 to 9/1, preferably 3/1 to 5/1.
Two embodiments of the solid-liquid phase reaction apparatus and the reaction method thereof according to the present invention will be described in detail below with reference to fig. 1 and 2. However, the scope of the present invention is not limited to those shown in FIGS. 1 and 2, and a solid-liquid phase reaction apparatus designed according to the idea of the present invention is within the scope of the present invention.
In the solid-liquid phase reaction device shown in fig. 1, a closed reactor shell 1 is an elliptic cylinder, a metal partition plate 2a with an opening is arranged in the closed reactor shell, a solid inlet 6 and a gas material outlet 8 are arranged at the top of the closed reactor shell, the metal partition plate 2a divides the inner space of the closed reactor shell 1 into an upper part and a lower part, the upper part is defined as a reaction area, the volume ratio of the upper part to the lower part is 5/1, a plurality of liquid inlets are arranged on the metal partition plate 2a, a pipeline connected with the liquid inlets penetrates through the bottom of the reactor shell, the gas material outlet 8 is connected with condensers 9 and 10, and emergency discharge tanks 12 and 13 are arranged at the bottom of the reactor shell. The solid inlet 6 is provided with a solid material feeding hopper, the lower part of the hopper is provided with an upper valve 7a and a lower valve 7b, a space is reserved between the two valves, the side wall of the space is provided with an inert gas purging port, and the purging port is connected with an inert gas purging pipeline 14 and an inert gas discharging pipeline 15.
Heated fatty alcohol is fed from line 16 to the reaction zone via liquid inlet A, B, C, D, E, F in metal partition 2 a. Irregular metal particles are added to the solid material feed hopper at the solid inlet 6, the upper valve 7a is closed, inert gas, preferably nitrogen, is introduced from the line 14 as purge gas to purge the metal particles, the purge gas is introduced from the inert gas discharge line 15 into the gas discharge line 27, and after purging is completed, the lower valve 7b is opened and the metal particles fall under gravity into the reaction zone. After the reaction starts, the liquid phase mixture of the alkoxide and the unreacted alcohol obtained by the reaction in the reactor is discharged from the product discharge line 18, and is circulated into the line 17 through the liquid phase material circulating pump (not shown in the figure) via the lines 19 and 20, and then enters the reaction zone from the liquid inlet on the metal partition plate 2a through the bottom of the reactor, so as to maintain the upper liquid layer of the metal partition plate 2a in a boiling state, and the boiling liquid layer increases the contact between the metal particles and the alcohol, thereby increasing the reaction rate and simultaneously dispersing the generated alkoxide rapidly and uniformly in the liquid phase material in the reactor. Hydrogen generated by the reaction of the fatty alcohol and the metal and alcohol vapor generated by exothermic evaporation are discharged from a gas phase material discharge port 8 at the top of the reactor, enter a condenser 9 and a condenser 10 through a pipeline 25, and return to the pipeline 16 from a pipeline 24a and a pipeline 24b after the alcohol vapor is condensed, and return to the reactor through a pipeline 17. The hydrogen passes through the flow meter 11 and exits the reactor system via line 27. The reaction product metal alkoxide compound and a portion of the unreacted alcohol are removed from line 18 via line 19, a portion being returned to the reactor via line 20 and another portion being withdrawn from the reactor via line 21.
In the solid-liquid phase reactor shown in fig. 2, a closed reactor shell 1 is an elliptic cylinder, a fixed sleeve 2b with an upper opening, a side part and a bottom part provided with open holes is arranged in the closed reactor shell 1, a solid inlet 6 and a gas phase material outlet 8 are arranged at the top part, the fixed sleeve 2b divides the internal space of the closed reactor shell 1 into an inner part and an outer part, the inside of the fixed sleeve 2b is defined as a reaction area, the volume ratio of the inner part to the outer part is 5/1, the upper part, the side wall and the bottom part of the reactor shell 1 are provided with a plurality of liquid inlets, and the gas phase material outlet 8 is connected with condensers 9 and 10. The bottom of the reactor shell is provided with emergency discharge tanks 12 and 13. The solid inlet 6 is provided with a solid feeding hopper, an upper valve 7a and a lower valve 7b are arranged below the feeding hopper, a space is reserved between the two valves, the side wall of the space is provided with an inert gas purging port, and the purging port is connected with an inert gas purging pipeline 14 and an inert gas discharging pipeline 15.
Heated fatty alcohol is fed from line 16 through liquid inlets H (top), I (top), J (side), K (bottom), L (bottom) into the reaction zone. Solid material of irregular metal solid particles is added into a solid material feeding hopper of a solid inlet 6, an upper valve 7a is closed, inert gas, preferably nitrogen, is introduced from a pipeline 14 to purge the metal particles, the purge gas is discharged from an inert gas discharge pipeline 15, and after purging is finished, a lower valve 7b is opened, and the metal particles fall into a reaction area under the action of gravity. After the reaction was started, nitrogen gas was introduced into the reactor from stirring gas inlets a (side), b (side), c (bottom) and d (bottom) through line 29 by passing through gas compressor 31 from line 28 and stirring. Hydrogen generated by the reaction of the fatty alcohol and the metal and alcohol vapor generated by exothermic evaporation enter a condenser 9 and a condenser 10 from a gas phase material outlet 8 at the top of the reactor through a pipeline 25, the alcohol vapor is condensed and then flows back to the reactor through a pipeline 24a and a pipeline 24b and a pipeline 17, and the hydrogen is metered by a flowmeter 11 and then is discharged out of the device. The reaction product metal alkoxide compound and a portion of the unreacted alcohol are removed from line 18 and then passed through line 19, a portion being refluxed back to the reactor via line 20 and another portion being withdrawn from the reactor via line 21.
When the reaction is too violent due to operation reasons or other reasons, hydrogen is generated in a large amount, and the temperature in the reactor is rapidly increased, valves (not shown) on the pipeline 22 and the pipeline 23 are opened, so that the liquid-phase material in the reactor is rapidly discharged into the emergency material storage tanks 12 and 13, the reaction is rapidly stopped, and the circulating pump (not shown) on the pipeline 19 is stopped. After the danger is relieved, the liquid phase materials in the emergency material storage tanks 12 and 13 are returned to the reactor through pipelines 19 and 20 to continue the reaction. The valves on lines 22 and 23 entering the emergency storage tanks may be configured as automatic valves that correlate to the temperature within the reactor and the flow rate on the hydrogen flow meter 11, and when the temperature rises to an alarm value or the hydrogen flow rate increases to an alarm value, the valves automatically open to emergently discharge the liquid phase material into the emergency storage tanks 12 and 13.
Claims (12)
1. A solid-liquid phase reaction device comprises a closed reactor shell (1) and a component which is arranged in the closed reactor shell and used for limiting a reaction area, wherein a solid inlet (6) and a gas phase material outlet (8) are arranged at the top of the closed reactor shell, a liquid inlet is arranged at the bottom and/or the side wall of the reactor shell, a solid feeding hopper is arranged on the solid inlet (6) of the device, an upper valve (7 a) and a lower valve (7 b) are arranged at the lower part of the hopper, a space is reserved between the two valves, and an inert gas purging port is arranged on the side wall of the space;
the component for limiting the reaction area is a metal partition plate (2a) with an opening, the metal partition plate (2a) divides the interior of the closed reactor shell (1) into an upper part and a lower part, a plurality of liquid inlets are arranged on the metal partition plate (2a), pipelines connected with the liquid inlets penetrate through the bottom of the closed reactor shell (1), and the average diameter of the opening on the metal partition plate (2a) is 0.5-20 mm.
2. The device of claim 1, wherein the volume ratio of the upper portion to the lower portion is 1/1 to 9/1.
3. The apparatus according to claim 1, wherein the means for delimiting the reaction zone is a fixing sleeve (2b) provided with openings at the upper opening, the sides and the bottom, the fixing sleeve (2b) dividing the interior of the closed reactor shell (1) into an inner part and an outer part, the average diameter of the openings on the fixing sleeve (2b) being 0.5-20 mm.
4. An apparatus according to claim 3, characterized in that the bottom and/or the side of the closed reactor shell (1) is provided with an inlet for stirring gas.
5. The device according to claim 3 or 4, wherein the volume ratio of the inner part to the outer part is 9/1 to 1/3.
6. The device of claim 5, wherein the volume ratio of the inner portion to the outer portion is 5/1 to 1/1.
7. An apparatus according to any one of claims 1-3, further comprising one or more emergency storage tanks in communication with the bottom of the closed reactor shell (1).
8. An apparatus according to any one of claims 1-3, characterized in that the apparatus further comprises a condenser, which is in communication with the discharge opening (8) for the gaseous phase material, which is arranged in the upper part of the closed reactor shell (1).
9. The method for producing a metal alkoxide compound using the solid-liquid phase reaction apparatus as set forth in any one of claims 1 to 3, wherein an aliphatic alcohol is fed through the liquid inlet, and a metal reactant is fed through the solid inlet, and the aliphatic alcohol and the metal reactant are brought into contact with each other in the reaction zone.
10. The method of claim 9, wherein the fatty alcohol is C1To C12The metal reactant is at least one of magnesium, aluminum, zinc, and zirconium.
11. The method of claim 9, wherein the particle size of the metal reactant is 3-20 cm.
12. The process according to claim 9, wherein a portion of the liquid phase material withdrawn from the closed reactor shell is recycled back to the reactor, the mass ratio of recycled material to withdrawn material being from 1/1 to 9/1.
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Citations (4)
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|---|---|---|---|---|
| US4590289A (en) * | 1982-12-04 | 1986-05-20 | Condea Chemie Gmbh | Process and apparatus for producing aluminium alkoxides |
| CN1162931A (en) * | 1994-11-08 | 1997-10-22 | Rwe-Dea矿物油化学有限公司 | Device for bringing pourable solids into contact with gases or liquids |
| CN1172098A (en) * | 1996-01-15 | 1998-02-04 | 塔尔努夫氮化物工厂 | Method and equipment for oxidation of cyclohexane and decomposition of cyclohexyl hydroperoxide |
| CN101426571A (en) * | 2006-04-07 | 2009-05-06 | 格特·艾伯特 | Apparatus and method for dissolving solids in liquids |
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2016
- 2016-07-29 CN CN201610616535.0A patent/CN107661734B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4590289A (en) * | 1982-12-04 | 1986-05-20 | Condea Chemie Gmbh | Process and apparatus for producing aluminium alkoxides |
| CN1162931A (en) * | 1994-11-08 | 1997-10-22 | Rwe-Dea矿物油化学有限公司 | Device for bringing pourable solids into contact with gases or liquids |
| CN1172098A (en) * | 1996-01-15 | 1998-02-04 | 塔尔努夫氮化物工厂 | Method and equipment for oxidation of cyclohexane and decomposition of cyclohexyl hydroperoxide |
| CN101426571A (en) * | 2006-04-07 | 2009-05-06 | 格特·艾伯特 | Apparatus and method for dissolving solids in liquids |
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