CN113117612A - Gas-liquid continuous reaction crystallization device - Google Patents
Gas-liquid continuous reaction crystallization device Download PDFInfo
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- CN113117612A CN113117612A CN202110475110.3A CN202110475110A CN113117612A CN 113117612 A CN113117612 A CN 113117612A CN 202110475110 A CN202110475110 A CN 202110475110A CN 113117612 A CN113117612 A CN 113117612A
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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
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
- B01J8/38—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it
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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
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1845—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with particles moving upwards while fluidised
- B01J8/1863—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with particles moving upwards while fluidised followed by a downward movement outside the reactor and subsequently re-entering it
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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
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1872—Details of the fluidised bed reactor
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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
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
- B01J8/22—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid
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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
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
- B01J8/26—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with two or more fluidised beds, e.g. reactor and regeneration installations
- B01J8/28—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with two or more fluidised beds, e.g. reactor and regeneration installations the one above the other
- B01J8/30—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with two or more fluidised beds, e.g. reactor and regeneration installations the one above the other the edge of a lower bed projecting beyond the edge of the superjacent bed
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- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00548—Flow
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- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
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- B01J2208/00628—Controlling the composition of the reactive mixture
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- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00743—Feeding or discharging of solids
- B01J2208/00769—Details of feeding or discharging
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00796—Details of the reactor or of the particulate material
- B01J2208/00823—Mixing elements
- B01J2208/00858—Moving elements
- B01J2208/00867—Moving elements inside the bed, e.g. rotary mixer
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- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00796—Details of the reactor or of the particulate material
- B01J2208/00946—Features relating to the reactants or products
- B01J2208/00955—Sampling of the particulate material, the reactants or the products
- B01J2208/00982—Particulate material
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Abstract
The invention discloses a device for gas-liquid continuous reaction crystallization, which comprises a reactor and a separator, wherein a gas distributor, a guide cylinder, a push type stirrer, a baffling baffle and a circulating liquid outlet pipe are arranged in the reactor; the gas reactant inlet pipe enters the inside of the reactor and is connected with the gas distributor, the gas distributor is positioned right above the guide cylinder, blades of the propelling stirrer are positioned inside the guide cylinder, the baffle plate is positioned right below the guide cylinder, the propelling stirring paddle is used for guiding liquid downwards at the central position of the guide cylinder, the baffle plate is used for turning the liquid back to the upper part of the reactor from the outside of the guide cylinder to enter the guide cylinder, so that the internal circulation of the reactor is formed, and the material exchange between the reactor and the separator forms the external circulation. The device is favorable for reducing the agglomeration of solid particles, reducing the content of liquid reactants and products wrapped by the solid particles, promoting the conversion of the liquid reactants and improving the recovery rate of the liquid products.
Description
Technical Field
The invention relates to an industrial special device which utilizes fluid flow, solid particle sedimentation and particle sorting reflux to reduce solid agglomeration obtained by reaction crystallization and reduce wrapped liquid-phase reactants so as to promote the liquid-phase reactants to be completely converted into products, and is applied to processes with gas consumption and solid generation at the same time, including related processes in chemical engineering, biological engineering, pharmacy and environmental protection. The invention particularly relates to a reaction device for gas-liquid continuous reaction crystallization.
Background
Gas-liquid reaction crystallization processes are important reaction processes, and gas reactants and liquid reactants (solute and solvent) are contacted at a gas-liquid interface to form solid particles and possibly form liquid products. The existing gas-liquid reaction crystallization technology makes a lot of designs and researches on the shape of the obtained solid particles, but the problems that the unreacted liquid reactant or liquid product is wrapped by the agglomerates formed by the solid particles and the like are seldom involved. Especially, inorganic salt solid produced in an organic reaction system often forms micron-sized solid particles and has a higher agglomeration tendency because the inorganic salt solid is often extremely low in solubility in a liquid phase, so that loose solid agglomerates are formed. If a large amount of liquid reactants and products are absorbed and coated in the agglomerate, great difficulty is brought to the conversion rate of the liquid reactants and the recovery and treatment of the liquid products.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a gas-liquid continuous reaction crystallization device, so as to reduce the wrapping of solid particle groups on liquid in the reaction crystallization process, improve the conversion rate of liquid reactants and effectively simplify the subsequent liquid product recovery process and the post-treatment process of solid particles.
A crystallization device for gas-liquid continuous reaction comprises a reactor and a separator; the reactor is provided with a gas reactant feeding pipe, a liquid reactant feeding pipe and a turbid liquid return pipe of the separator as material input ports, and a slurry sampling port of the reactor as an output port; wherein the slurry extraction outlet of the reactor is sequentially connected with a circulating pump and a separator inlet pipe so as to be connected with a separator; the liquid reactant feeding pipe and the turbid liquid return pipe of the separator are combined and then connected with the circulating liquid outlet pipe; the inside of the reactor is provided with a gas distributor, a guide cylinder, a push type stirrer, a baffling baffle and a circulating liquid outlet pipe; the gas reactant inlet pipe enters the inside of the reactor and is connected with the gas distributor, the gas distributor is positioned right above the guide cylinder, blades of the propelling stirrer are positioned inside the guide cylinder, the propelling stirrer is connected with a motor arranged at the top of the reactor, a baffling baffle is positioned right below the guide cylinder, an outlet end of the circulating liquid outlet pipe is positioned below the baffling baffle, the propelling stirring paddle is used for guiding liquid downwards at the center of the guide cylinder, the baffling baffle is used for turning the liquid back to the upper part of the reactor from the outside of the guide cylinder to enter the guide cylinder, so that a reactor inner circulation is formed, and material exchange between the reactor and the separator forms an outer circulation.
The separator is divided into an upper part, a middle part and a lower part, wherein the diameter of the upper part for solid settlement is larger, the highest part of the upper part is provided with a clear liquid collecting outlet of the separator, the middle part is provided with the inlet pipe of the separator, and the funnel-shaped bottom end of the lower part is a turbid liquid outlet of the separator for discharging turbid liquid; a separator energy dissipation baffle plate for reducing the kinetic energy of the fluid is arranged in front of the inlet pipe of the separator, and a separator lower baffle plate and a separator upper baffle plate for intercepting solid particles are arranged at the upper part of the separator energy dissipation baffle plate; the turbid liquid outlet of the separator is connected with the flow divider, one branch of the flow divider is output through the circulating liquid outlet pipe, and the other branch of the flow divider is output through the product discharge pipe.
And the clear liquid extraction port of the separator is connected with a product discharge pipe.
The separator is a settler, a cyclone or a thickener.
The baffle plate is a conical surface, and the vertex angle is 100-170 degrees.
The reflux ratio of the flow divider is controlled to be 1-500.
The invention has the beneficial effects that:
1) the continuous feeding and discharging, the reaction device is added with external circulation, and the flow direction of the liquid returned circularly is from bottom to top, thus being beneficial to the suspension of solid particles in the reactor and avoiding the deposition and agglomeration.
2) The generated agglomerates are broken by a pump in external circulation, the slurry is primarily separated by a separator, solid agglomerates in the turbid liquid are broken again and then return to the reactor, and a clear liquid output device improves the utilization efficiency of the wrapped reactants.
3) The gas distributor is positioned above the liquid level, and the potential suck-back risk in the rapid reaction system is reduced.
4) A push type stirrer is adopted and matched with a guide cylinder, so that agglomeration of solids in the reaction process is inhibited.
Drawings
FIG. 1 is a schematic view of a gas-liquid continuous reaction crystallization apparatus.
In the figure: the device comprises a gas reactant feeding pipe 1, a liquid reactant feeding pipe 2, a reactor 3, a gas distributor 4, a guide cylinder 5, a propelling stirrer 6, a baffling baffle 7, a circulating liquid outlet pipe 8, a separator inlet pipe 9, a separator clear liquid outlet 10, a separator 11, a separator upper baffle 12, a separator lower baffle 13, a separator energy dissipation baffle 14, a reactor slurry extraction pipe 15, a separator turbid liquid outlet 16, a circulating pump 17, a separator turbid liquid return pipe 18, a flow divider 19 and a product discharge pipe 20.
Detailed Description
The invention is further illustrated below with reference to the figures and examples.
As shown in figure 1, the gas-liquid continuous reaction crystallization device comprises a reactor and a separator which are connected by a pump and a pipeline to form a circulation loop. The reactor 3 contains the components arranged in sequence: the gas distributor 4 to which the gaseous reactant feed 1 is connected is located in the reactor at a position below the liquid surface and close to the liquid surface. The guide shell 5 is arranged below the gas distributor 4 in the middle of the reactor, the push type stirrer 6 is arranged in the center of the guide shell 5, the baffle 7 is arranged below the guide shell, the circulating liquid outlet pipe 8 is arranged at the bottom of the reactor, the slurry outlet pipe 15 of the reactor is arranged below the liquid level of the upper part of the reactor and close to the liquid level area, and the upper edge of the slurry outlet pipe is higher than the gas distributor 4. The slurry in the reactor circularly flows under the conveying of the circulating pump and the stirring of the internal propelling stirrer, wherein the slurry in the guide cylinder flows from top to bottom, and the slurry outside the guide cylinder flows from bottom to top.
The circulating pump 17 has both functions of conveying the slurry and breaking the aggregates of the particles. The separator is a cylindrical structure with a large upper diameter and a small lower diameter, reaction slurry containing particles is input from a separator inlet pipe 9 at the middle lower part of the separator, and a separator energy dissipation baffle plate 14 is arranged at the front end of the separator to reduce the kinetic energy of liquid. The upper portion is provided with two department's slope baffles in separator 11, is separator upper baffle 12 and separator lower baffle 13 respectively, and the diameter of upper portion is bigger than inlet tube 9 department, further reduces the liquid velocity of flow, does benefit to and subsides. The low particle content clear liquid is withdrawn from the separator head separator clear liquid outlet 10. The lower part of the separator is of a cone-cylinder structure, turbid liquid with large solid content and large agglomerated particle size is discharged from a turbid liquid outlet 16 at the bottom of the separator, after being distributed by a flow divider 19, a part of the turbid liquid is conveyed by a turbid liquid return pipe 18 and is mixed with fresh liquid raw materials continuously input from a liquid reactant feeding pipe 2, and the mixture is returned to the bottom of the reactor by a circulating liquid outlet pipe 8, and a part of the turbid liquid is mixed with clear liquid output from a clear liquid collecting outlet 10 of the separator and is continuously conveyed to a subsequent working section by a product discharge pipe 20. The flow divider 19 can be adjusted to achieve a change in the ratio of the volumes of the two portions of liquid.
The guide shell 4 is a hollow cylinder with a conical cylinder at the upper part and a cylindrical cylinder at the lower part. The inner diameter of the lower cylindrical barrel is matched with the diameter of the stirrer blade, so that agglomerated particles can be broken by sufficient turbulence. The baffling baffle 7 below the guide cylinder is a conical side face, the angle of the vertex angle is 100-170 degrees, and the diameter of the bottom face is larger than the outer diameter of the lower end of the guide cylinder. The slurry extraction pipe 15 of the reactor is positioned in the upper part of the reactor close to the liquid level area, and the liquid extraction port at the upper part of the slurry extraction pipe is higher than the upper edge of the guide shell.
The flow divider 19 is a three-way valve capable of continuously adjusting the flow rate, and is used for adjusting the ratio of the slurry flow rate (reflux ratio) conveyed back to the reactor and output from the reaction device, and the parameters influence the utilization efficiency of gas and liquid in the reactor and the agglomeration degree of output particles. The reflux ratio is controlled to be generally 1 to 500.
The separator can adopt a simple settling structure in the figure, and can also adopt a suspension separator or a thickener according to the actual condition of the process. The reflux ratio should be adapted to the separation effect.
The reaction device can be designed with a heat exchange and heat preservation structure according to the requirements of the reaction process. Fluid flow control devices such as valves and conveying devices such as pumps are required to be installed in the pipelines according to actual requirements.
Example bench test reaction apparatus
The gas-liquid continuous reaction crystallization device is adopted to continuously produce hexamethyldisilazane, the reactant is trimethyl chlorosilane, the solvent is hexamethyldisiloxane, the gas participating in the reaction is pure ammonia, and the products are hexamethyldisilazane and solid ammonium chloride. The total volume of liquid in the device is 120mL, and the proportion of the volume of the fluid returning to the reactor and the volume of the fluid leaving the reaction device is controlled by 200 after the turbid liquid of the separator is split. The reaction temperature is controlled at 30 ℃, the input flow of ammonia gas is 150mL/min, the liquid reactant trimethylchlorosilane and hexamethyldisiloxane are mixed according to the volume ratio of 1: 4 and then input into the reaction device, the flow is 5mL/min, and the flow of liquid returned by the flow divider 19 to the reactor is controlled at 60L/h. After the hexamethyldisiloxane solvent is fed into the reactor from the liquid reactant feed line 2 to the operating level, the circulation pump 17 and the propeller stirrer 6 are turned on, and the flow divider 19 is adjusted to the appropriate reflux ratio. Ammonia gas was fed through gaseous reactant feed line 1, while liquid reactant was fed through liquid reactant feed line 2. The flow rate of the liquid output from the product discharge pipe 20 is adjusted to stabilize the volume of the liquid in the apparatus. And continuously collecting the slurry output by the product discharge pipe 20, and calculating the reactant conversion rate after the liquid component content is stable. The conversion rate of the reactant trimethylchlorosilane can reach more than 95 percent. The particle size distribution of the flowing ammonium chloride solid particles is detected by a laser particle sizer, and the average particle size of the particles is 36 mu m. After centrifugation of the solids in the output slurry, the weight of the coating liquid was determined to be 43% of the total weight of the solids. Under comparable conditions, the traditional batch kettle type reaction can obtain the average particle size of the solid particles of 92 mu m, and the weight of the obtained solid coating liquid accounts for 56 percent of the total weight of the solid. The device can obviously relieve the agglomeration phenomenon of solid particles, and simultaneously, the weight of the wrapping liquid is reduced to some extent.
| Device for measuring the position of a moving object | Average particle diameter | Weight ratio of wrapping liquid |
| The invention discloses a patent device | 36μm | 43% |
| Batch kettle type reactor | 92μm | 56% |
Claims (6)
1. A crystallization device for gas-liquid continuous reaction is characterized in that: comprises a reactor (3) and a separator (11); the reactor (3) is provided with a gas reactant feeding pipe (1), a liquid reactant feeding pipe (2) and a separator turbid liquid return pipe (18) as material input ports, and a reactor slurry extraction port (15) as an output port; wherein the slurry extraction outlet (15) of the reactor is sequentially connected with a circulating pump (17) and a separator inlet pipe (9) so as to be connected with a separator (11); the liquid reactant feeding pipe (2) and the turbid liquid return pipe (18) of the separator are combined and then connected with the circulating liquid outlet pipe (8); a gas distributor (4), a guide cylinder (5), a push type stirrer (6), a baffling baffle (7) and a circulating liquid outlet pipe (8) are arranged in the reactor (3); the gas reactant feeding pipe (1) enters the reactor (3) and is connected with the gas distributor (4), the gas distributor (4) is positioned right above the guide cylinder (5), the blade of the push-type stirrer (6) is positioned inside the guide cylinder (5), the push-type stirrer (6) is connected with the motor arranged at the top of the reactor (3), a baffling baffle (7) is positioned right below the guide cylinder (5), the outlet end of the circulating liquid outlet pipe (8) is positioned below the baffling baffle (7), the push-type stirring paddle (6) is used for guiding liquid downwards at the central position of the guide cylinder (5), the baffling baffle (7) is used for bending the liquid from the outside of the guide cylinder (5) back to the upper part of the reactor to enter the guide cylinder (5), thus forming an internal circulation in the reactor (3) and an external circulation in the material exchange between the reactor (3) and the separator (11).
2. The gas-liquid continuous reaction crystallization apparatus according to claim 1, characterized in that: the separator (11) is divided into an upper part, a middle part and a lower part, wherein the diameter of the upper part for settling solids is larger, the highest part of the upper part is provided with a clear liquid collecting outlet (10) of the separator, the middle part is provided with the inlet pipe (9) of the separator, and the funnel-shaped bottom end of the lower part is a turbid liquid outlet (16) of the separator for discharging turbid liquid; a separator energy dissipation baffle plate (14) for reducing the kinetic energy of the fluid is arranged in front of the separator inlet pipe (9), and a separator lower baffle plate (12) and a separator upper baffle plate (13) for intercepting solid particles are arranged at the upper part of the separator energy dissipation baffle plate; the turbid liquid outlet (16) of the separator is connected with a flow divider (19), one branch of the flow divider is output through a circulating liquid outlet pipe (8), and the other branch of the flow divider is output through a product discharge pipe (20).
3. The gas-liquid continuous reaction crystallization apparatus according to claim 2, characterized in that: the clear liquid extraction port (10) of the separator is connected with a product discharge pipe (20).
4. The gas-liquid continuous reaction crystallization apparatus according to claim 1, characterized in that: the separator (11) is a settler, a cyclone or a thickener.
5. The gas-liquid continuous reaction crystallization apparatus according to claim 1, characterized in that: the baffle plate (7) is a conical surface, and the vertex angle is 100-170 degrees.
6. The gas-liquid continuous reaction crystallization apparatus according to claim 1, characterized in that: the reflux ratio of the flow divider (19) is controlled to be 1-500.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110475110.3A CN113117612A (en) | 2021-04-29 | 2021-04-29 | Gas-liquid continuous reaction crystallization device |
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| CN202110475110.3A CN113117612A (en) | 2021-04-29 | 2021-04-29 | Gas-liquid continuous reaction crystallization device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115043763A (en) * | 2022-06-14 | 2022-09-13 | 天津大学 | Gas-liquid continuous crystallization method of DL-methionine |
| CN115155490A (en) * | 2022-06-16 | 2022-10-11 | 安徽广信农化股份有限公司 | Continuous preparation device for reducing unit consumption of isocyanate solvent and preparation method thereof |
-
2021
- 2021-04-29 CN CN202110475110.3A patent/CN113117612A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115043763A (en) * | 2022-06-14 | 2022-09-13 | 天津大学 | Gas-liquid continuous crystallization method of DL-methionine |
| CN115043763B (en) * | 2022-06-14 | 2024-04-05 | 天津大学 | Gas-liquid continuous crystallization method of DL-methionine |
| CN115155490A (en) * | 2022-06-16 | 2022-10-11 | 安徽广信农化股份有限公司 | Continuous preparation device for reducing unit consumption of isocyanate solvent and preparation method thereof |
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