CN116173867A - Jacket type temperature-controllable continuous full-mixing stirring reactor - Google Patents
Jacket type temperature-controllable continuous full-mixing stirring reactor Download PDFInfo
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- CN116173867A CN116173867A CN202211692162.7A CN202211692162A CN116173867A CN 116173867 A CN116173867 A CN 116173867A CN 202211692162 A CN202211692162 A CN 202211692162A CN 116173867 A CN116173867 A CN 116173867A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/14—Production of inert gas mixtures; Use of inert gases in general
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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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1862—Stationary reactors having moving elements inside placed in series
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
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Abstract
The invention discloses a jacketed type temperature-controllable continuous full-mixing stirring reactor which comprises a shell, a reaction kettle set, a circulating oil bath seal groove and a temperature control system, wherein the circulating oil bath seal groove is fixedly arranged in the shell and is electrically connected with the temperature control system, the reaction kettle set is detachably arranged in the circulating oil bath seal groove, and the reaction kettle set comprises a plurality of reaction kettles which are connected in series through transfer pipelines. The invention can ensure stable amplification of the reaction and simultaneously prevent the problem of device blockage caused by intermediates or side reaction products, so that the industrial amplified production process is stable, safe and controllable and has higher yield.
Description
Technical Field
The invention relates to the technical field of preparation encapsulation methods and equipment, in particular to a jacketed type temperature-controllable continuous full-mixing stirring reactor.
Background
The metallization organic reaction of the metal reagent is a chemical reaction frequently used in fine chemical production, and the reaction mechanism is as follows:
the reactant and the metal reagent are subjected to lithiation reaction, lithium halide exchange, grignard reaction and the like at low temperature to generate hydrocarbon lithium or hydrocarbon magnesium compound, and then react with the active hydrogen compound to obtain the corresponding derivative. The reaction rate of the aforementioned reaction is extremely fast, often in the order of seconds or minutes.
In the prior art, a batch reactor is generally used for the metallization organic reaction of the metal reagent. In the patent document with the publication number of CN111187200A, an intermittent lithiation hydrogen-extracting reaction is provided for synthesizing lometapi-D8, and the reaction provided by the method is influenced by the change of conditions to generate obvious amplification effect after being amplified by a reaction kettle, and the problems of unstable intermediates, influence on yield, limited production capacity and the like are caused; in the patent document with publication number of CN103028356A, an aromatic heterocyclic lithium halogen exchange reaction device of a microreactor is provided, the reaction rate is improved, the reaction is effectively controlled to be completed within a few seconds, the product yield is improved, the problem of amplification effect is avoided, however, the lithium halogen exchange reaction under the reaction device does not solve the problem that a reaction intermediate is easy to further react with a metal reagent to cause device blockage, and therefore long-period production is difficult, and the industrial applicability is poor.
Therefore, in the art, there is a need to develop a reaction device for a metallization organic reaction with a high reaction rate, which has wide applicability, can prevent the device blockage caused by side reaction products while ensuring stable amplification of the reaction, and thus, the industrial amplified production process is stable, safe and controllable, and has high yield.
Disclosure of Invention
In order to solve the technical problems, the invention provides a jacketed type temperature-controllable continuous total-mixing stirring reactor which comprises a shell, a reaction kettle sleeve group, a circulating oil bath sealing groove and a temperature control system, wherein the circulating oil bath sealing groove is fixedly arranged in the shell and is electrically connected with the temperature control system, the reaction kettle sleeve group is detachably arranged in the circulating oil bath sealing groove, and the reaction kettle sleeve group comprises a plurality of reaction kettles which are connected in series through transfer pipelines. In a specific embodiment, the volume, quantity and materials of the reaction kettles can be adjusted according to the characteristics of reactants, the reaction time, the temperature and the like, and the unused reaction kettles are sealed in the left space of the upper cover of the circulating oil bath sealing groove, wherein the sealing comprises but is not limited to a pagoda head sealing.
Specifically, the temperature control system is an external flow type temperature control system, the purpose of controlling the temperature of the reaction system is achieved by controlling the temperature of the oil bath, and the external flow type temperature control system can control the temperature of the reaction system to be-80-100 ℃.
Specifically, the circulating oil bath seal groove comprises a detachable upper cover, and the reaction kettle sleeve group is fixedly connected with the upper cover through a flange.
Specifically, the shape of the reaction kettle comprises, but is not limited to, a cylindrical shape or a round bottom shape, and the shape of the circulating oil bath seal groove comprises, but is not limited to, a cube or a cylinder.
Specifically, the reaction kettle set comprises at least four reaction kettles, and the volume of the reaction kettles is not more than 1000mL.
Preferably, the reaction kettle set comprises 1 reaction kettle with the volume of not more than 1000mL and 8 reaction kettles with the volume of not more than 250 mL.
Specifically, each reaction kettle is internally provided with a plurality of reaction columns and 1 thermocouple, and the reaction columns and the thermocouples are fixedly arranged in the reaction kettle through an upper cover of the reaction kettle.
Specifically, the material of the reaction kettle is selected from one of stainless steel, hastelloy or glass.
Specifically, the reaction kettle is a magnetic stirring reaction kettle or a mechanical stirring reaction kettle.
Specifically, the material of the transfer pipeline is selected from stainless steel, hastelloy or soluble polytetrafluoroethylene PFA.
Specifically, the feed inlet of transfer pipeline is located reation kettle's bottom, the discharge gate of transfer pipeline is located reation kettle's top.
Specifically, the pressure-resistant bearing ranges of the reaction kettle and the circulating oil bath seal groove are at least 10bar.
Specifically, the reaction kettle and the transfer pipeline are immersed in the medium of the circulating oil bath seal groove.
Specifically, inert gas is introduced into the reaction kettle sleeve group, and the inert gas is used for providing driving force for a reaction system.
Specifically, the inert gas includes nitrogen or argon.
Specifically, the jacketed type temperature-controllable continuous total-mixing stirring reactor further comprises a raw material tank, a reagent tank, a feed pump, a product storage tank and other production matching devices, wherein the feed pump is preferably a peristaltic pump.
The invention also provides a method for carrying out the metallization organic reaction of the metal reagent by using the jacketed type temperature-controllable continuous total-mixing stirring reactor, which comprises the following steps:
s1, preparing reaction raw materials and metal reagents, and adding the reaction raw materials and the metal reagents into a reaction kettle sleeve group of the jacketed type temperature-controllable continuous full-mixing stirring reactor;
s2, setting the temperature of an external flow type temperature control system as the temperature required by the reaction, and carrying out a metallization organic reaction.
Compared with the prior art, the invention has the beneficial effects that:
1. the jacketed type temperature-controllable continuous total-mixing stirring reactor provided by the invention selects the reaction kettle with smaller volume as the first mixing reaction kettle, and because the volume of a single reaction kettle is small (< 250 mL), the influence of back mixing on the selectivity/conversion rate of a reaction system is avoided, so that the metallized organic reaction process of a metal reagent has no obvious change in the amplifying process, and the amplifying effect is avoided; in addition, the single reaction kettle with a small volume has larger heat transfer specific surface area, which is beneficial to controlling the internal temperature of the reaction kettle.
2. The jacketed type temperature-controllable continuous total-mixing stirring reactor provided by the invention is different from a traditional intermittent reaction kettle, adopts an integrated small-volume reaction kettle series connection mode, and adopts gravity potential difference or inert gas as motive power of a transfer reaction system to construct a flow chemical continuous module production mode, so that the problem that a reaction pipeline is blocked by side reaction products due to unstable intermediates is effectively prevented, and the settling of solid particles is avoided due to the arrangement mode of the transfer pipe and higher linear flow rate, so that the production cycle can be prolonged, the production cost is saved and the production efficiency is improved while the amplification production is facilitated;
3. the jacketed type temperature-controllable continuous total-mixing stirring reactor provided by the invention can realize the metallized organic reaction amplification production of metal reagents, and is widely applied to the construction of aromatic or heterocyclic compounds with complex structures to synthesize various drug molecules with important physiological effects.
Drawings
FIG. 1 is a schematic top view of one embodiment of a jacketed temperature-controllable continuous mix stirred reactor of the present invention;
FIG. 2 is a schematic side view of one embodiment of a jacketed temperature-controllable continuous mix stirred reactor of the present invention;
in the figure, 1, a reaction kettle sleeve group; 2. a circulating oil bath seal groove; 3. a magnet; 4. a reaction kettle upper cover; 5. a thermocouple; 6. a reaction column; 7. and (5) transferring the pipeline.
Detailed Description
The following description of the present invention will be made clearly and fully, and it is apparent that the embodiments described are some, but not all, of the embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. Materials, instruments, reagents and the like used in the following examples are commercially available unless otherwise specified. The technical means used in the examples, unless otherwise specified, are conventional means well known to those skilled in the art.
The structures, proportions, sizes, etc. shown in the drawings herein are shown in detail, and should not be construed as limiting the scope of the invention, since it is intended that all changes in structure, proportion, or adjustment of size be included in the scope of the invention without affecting the efficiency or achievement thereof, and terms such as "upper", "lower", "left", "right", "middle", and "one" are used for descriptive purposes only and are not intended to limit the scope of the invention.
Example 1
The jacket type temperature-controllable continuous total-mixing stirring reactor comprises a shell, a reaction kettle sleeve group 1, a circulating oil bath sealing groove 2 and a temperature control system, wherein the circulating oil bath sealing groove 2 is fixedly arranged in the shell, the circulating oil bath sealing groove 2 is electrically connected with the temperature control system, the reaction kettle sleeve group 1 is detachably arranged in the circulating oil bath sealing groove 2, and the reaction kettle sleeve group 1 comprises a plurality of reaction kettles which are connected in series through transfer pipelines 7.
In a specific embodiment, the volume, quantity and materials of the reaction kettles can be adjusted according to the characteristics of reactants, reaction time, temperature and other conditions, and the unused reaction kettles are sealed in the left space covered on the circulating oil bath sealing groove 2, wherein the sealing comprises but is not limited to pagoda head sealing.
As shown in FIG. 1, the top view of the jacketed type temperature-controllable continuous total-mixing stirring reactor of the reaction kettle sleeve group 1 is formed by adopting 1 reaction kettle with the volume of not more than 1000mL and 8 reaction kettles with the volume of not more than 250 mL; as shown in FIG. 2, a side view of a jacketed type temperature-controllable continuous total mixing stirred reactor of a reaction kettle set 1 composed of 4 reaction kettles with volumes not exceeding 250mL was shown.
The temperature control system is an external flow type temperature control system, the purpose of controlling the temperature of the reaction system is achieved by controlling the temperature of the oil bath, and the external flow type temperature control system can control the temperature of the reaction system to be-80-100 ℃.
The circulating oil bath seal groove 2 comprises a detachable upper cover, and the reaction kettle sleeve group 1 is fixedly connected with the upper cover through a flange.
The shape of the reaction vessel includes, but is not limited to, a cylindrical shape or a round bottom shape, and the shape of the circulating oil bath seal groove 2 includes, but is not limited to, a square or a cylinder.
The reaction kettle sleeve group 1 comprises at least four reaction kettles, and the volume of the reaction kettles is not more than 1000mL.
The reaction kettle sleeve 1 comprises 1 reaction kettle with the volume not exceeding 1000mL and 8 reaction kettles with the volume not exceeding 250 mL.
A plurality of reaction columns 6 and 1 thermocouple 5 are arranged in each reaction kettle, and the reaction columns 6 and the thermocouples 5 are fixedly arranged in the reaction kettles through the upper covers 4 of the reaction kettles.
The material of the reaction kettle is one of stainless steel, hastelloy or glass.
The reaction kettle is a magnetic stirring reaction kettle or a mechanical stirring reaction kettle, and when the magnetic stirring reaction kettle is adopted, a magneton 3 is arranged at the bottom in the reaction kettle.
The material of the transfer pipe 7 is selected from stainless steel, hastelloy or soluble polytetrafluoroethylene PFA.
The feed inlet of transfer pipeline 7 is located reation kettle's bottom, and the discharge gate of transfer pipeline 7 is located reation kettle's top.
The pressure-resistant bearing ranges of the reaction kettle and the circulating oil bath seal groove 2 are at least 10bar.
Both the reaction kettle and the transfer pipeline 7 are immersed in the medium of the circulating oil bath seal groove 2.
Inert gas is introduced into the reaction kettle sleeve group 1, and the inert gas is used for providing driving force for a reaction system.
The inert gas includes nitrogen or argon.
The jacketed type temperature-controllable continuous total-mixing stirring reactor also comprises production matching devices such as a raw material tank, a reagent tank, a feed pump, a product storage tank and the like, wherein the feed pump is preferably a peristaltic pump.
The invention also provides a method for carrying out the metallization organic reaction of the metal reagent by using the jacketed type temperature-controllable continuous total-mixing stirring reactor, which comprises the following steps:
s1, preparing reaction raw materials and metal reagents, and adding the reaction raw materials and the metal reagents into a reaction kettle sleeve group 1 of the jacketed type temperature-controllable continuous full-mixing stirring reactor;
s2, setting the temperature of an external flow type temperature control system as the temperature required by the reaction, and carrying out a metallization organic reaction.
In examples two to five, specific embodiments for synthesizing 2-acetyl-5-bromopyridine, 2, 6-difluoro-4-iodopyridine and 4-methoxy-benzaldehyde by using the jacketed type temperature-controllable continuous total mixing stirring reactor provided by the invention will be shown.
Example two
2, 5-dibromopyridine (100 g,0.42mol,1.0 eq.) was dissolved in 1000mL (10V) toluene and the solution was named solution A after purging. N-butyllithium n-hexane solution (195 mL,1.15 eq.) with a specification of 2.5M was designated as solution B for use. N, N-dimethylacetamide (66 g,1.8 eq.) was dissolved in 500mL (5V) toluene and the solution was named solution C after purging. The 27wt% aqueous ammonium chloride solution was designated as solution D for use.
A set of jacketed type temperature-controllable continuous total-mixing stirring reactor is assembled as a reaction device, and the specific specification is as follows: 4 glass reaction columns with height-to-diameter ratio of 3:1 (inner diameter of 1.5 cm), wherein the inlet of each reaction column is 0.5cm away from the bottom, the outlet of each reaction column is 2cm away from the bottom, the effective volume is 3mL, and the connecting pipe is a 1/4inch PFA hose. The liquid in the reaction column is mixed by magnetic stirring, and the mixture transfer between the columns is pushed by nitrogen. The circulating oil bath sealing groove is connected with a refrigerating and heating temperature control system, and the temperature is controlled to be between-40 ℃ and-20 ℃.
The solution A, B, C, D is conveyed by peristaltic pumps, the flow rates are respectively set to 7.7mL/min, 1.4mL/min, 4.2mL/min and 5.8mL/min, the solution A and the solution B enter a glass reaction column after precooling, the solution C enters another glass reaction column after precooling, the solution D enters a quenching kettle, isopropanol is added to replace solvent toluene after split-phase concentration, and then 200mL of water is added to crystallize, so that 61g of 2-acetyl-5-bromopyridine is obtained, and the yield is 72%. The capacity of the reaction device was 1 kg/day.
Example 2
2, 5-dibromopyridine (5000 g,21.1mol,1.0 eq.) was dissolved in 50L (10V) toluene and the solution was named solution A after purging. N-butyllithium n-hexane solution (9.7L, 1.15 eq.) having a specification of 2.5M was designated as solution B for use. N, N-dimethylacetamide (3310 g,1.8 eq.) was dissolved in 25L (5V) toluene and the solution was named solution C after purging. The 27wt% aqueous ammonium chloride solution was designated as solution D for use.
A set of jacketed type temperature-controllable continuous total-mixing stirring reactor is assembled as a reaction device, and the specific specification is as follows: 4 stainless steel reaction columns with height-to-diameter ratio of 3:1 (inner diameter of 4 cm), wherein the inlet of each reaction column is 2cm away from the bottom, the outlet of each reaction column is 8cm away from the bottom, the effective volume is 100mL, and the connecting pipe is a 1/4inch stainless steel pipe. The liquid in the reaction column is mixed by magnetic stirring, and the mixture transfer between the columns is pushed by nitrogen. The circulating oil bath sealing groove is connected with a refrigerating and heating temperature control system, and the temperature is controlled to be between 50 ℃ below zero and 20 ℃ below zero.
The solution A, B, C, D is conveyed by peristaltic pumps, the flow rates are respectively set to 255mL/min, 47mL/min, 140mL/min and 193mL/min, the solution A and the solution B enter a stainless steel reaction column after precooling, the solution C enters another stainless steel reaction column after precooling, the solution D enters a quenching kettle, isopropanol is added to replace solvent toluene after split-phase concentration, and then 10L of water is added to crystallize, thereby obtaining 3123g of 2-acetyl-5-bromopyridine, and the yield is 74%. The capacity of the reaction device was 35 kg/day.
Example 3
2, 6-difluoropyridine (5000 g,43.4mol,1.0 eq.) was dissolved in 100L (20V) tetrahydrofuran and the solution was named solution A after the solution was taken out for use. N-butyllithium n-hexane solution (18 l,1.04 eq.) with a specification of 2.5M was named solution B for use. Elemental iodine (11245 g,1.02 eq.) was dissolved in 50L (10V) tetrahydrofuran and the solution was named solution C after purging. The aqueous sodium sulfite solution with the specification of 6wt% is named solution D for use.
A set of jacketed type temperature-controllable continuous total-mixing stirring reactor is assembled as a reaction device, and the specific specification is as follows: 2 stainless steel reaction columns with the height-diameter ratio of 3:1 (inner diameter of 4 cm) and 2 stainless steel reaction columns with the height-diameter ratio of 2:1 (inner diameter of 6 cm), wherein the inlet of each reaction column is 2cm away from the bottom, the outlet of each reaction column is 8cm away from the bottom, the effective volume is 100mL and 225mL, and the connecting pipe is a 1/4inch stainless steel pipe. The liquid in the reaction column is mixed by magnetic stirring, and the mixture transfer between the columns is pushed by nitrogen. The circulating oil bath sealing groove is connected with a refrigerating and heating temperature control system, and the temperature is controlled to be between 70 ℃ below zero and 30 ℃ below zero.
The solution A, B, C, D is conveyed by peristaltic pumps, the flow rates are respectively set to be 85.4mL/min, 14.6mL/min, 50.1mL/min and 43.2mL/min, the solution A and the solution B enter a stainless steel reaction column after precooling, the solution C enters another stainless steel reaction column after precooling, the solution D enters a quenching kettle, methyl tertiary butyl ether is added to replace solvent tetrahydrofuran after phase separation and concentration, and 2, 6-difluoro-4-iodopyridine solution is obtained, and the yield is 92%. The capacity of the reaction device was 6 kg/day.
Example 4
2, 6-difluoropyridine (5000 g,43.4mol,1.0 eq.) was dissolved in 100L (20V) tetrahydrofuran and the solution was named solution A after the solution was taken out for use. N-butyllithium n-hexane solution (18 l,1.04 eq.) with a specification of 2.5M was named solution B for use. Elemental iodine (11245 g,1.02 eq.) was dissolved in 50L (10V) tetrahydrofuran and the solution was named solution C after purging. The aqueous sodium sulfite solution with the specification of 6wt% is named solution D for use.
A set of jacketed type temperature-controllable continuous total-mixing stirring reactor is assembled as a reaction device, and the specific specification is as follows: 4 stainless steel reaction columns with the height-diameter ratio of 2:1 (inner diameter of 6 cm), 1 stainless steel reaction column with the height-diameter ratio of 1:1 (inner diameter of 10 cm), wherein the inlet of the reaction column is 2cm away from the bottom, the outlet of the reaction column is 8cm away from the bottom, the effective volume is 225mL and 600mL, and the connecting pipe is a 1/4inch stainless steel pipe. The liquid in the reaction column is mixed by magnetic stirring, and the mixture transfer between the columns is pushed by nitrogen. The circulating oil bath sealing groove is connected with a refrigerating and heating temperature control system, and the temperature is controlled to be between 70 ℃ below zero and 30 ℃ below zero.
The solution A, B, C, D is conveyed by peristaltic pumps, the flow rates are respectively set to 240mL/min, 41mL/min, 141mL/min and 121mL/min, the solution A and the solution B enter a stainless steel reaction column after precooling, the solution C enters another stainless steel reaction column after precooling, the solution D enters a quenching kettle, methyl tertiary butyl ether is added to replace solvent tetrahydrofuran after split-phase concentration, and the 2, 6-difluoro-4-iodopyridine solution is obtained with the yield of 93%. The capacity of the reaction device was 16 kg/day.
Example 5
1-bromo-4-methoxy-benzene (5000 g,26.7mol,1.0 eq.) was dissolved in 50L (10V) tetrahydrofuran and the solution was named solution A after the solution was cleared for use. N-butyllithium n-hexane solution (13L, 1.2 eq.) having a specification of 2.5M was designated as solution B for use. N, N-dimethylformamide (3910 g,2.0 eq.) was dissolved in 25L (5V) tetrahydrofuran and the solution was named solution C after purging. The 27wt% aqueous ammonium chloride solution was designated as solution D for use.
A set of jacketed type temperature-controllable continuous total-mixing stirring reactor is assembled as a reaction device, and the specific specification is as follows: 4 stainless steel reaction columns with height-to-diameter ratio of 2:1 (inner diameter of 6 cm), wherein the inlet of each reaction column is 2cm away from the bottom, the outlet of each reaction column is 8cm away from the bottom, the effective volume is 225mL, and the connecting pipe is a 1/4inch stainless steel pipe. The liquid in the reaction column is mixed by magnetic stirring, and the mixture transfer between the columns is pushed by nitrogen. The circulating oil bath sealing groove is connected with a refrigerating and heating temperature control system, and the temperature is controlled to be between 70 ℃ below zero and 30 ℃ below zero.
The solution A, B, C, D is conveyed by peristaltic pumps, the flow rates are respectively set to 366mL/min, 84mL/min, 191mL/min and 279mL/min, the solution A and the solution B enter a stainless steel reaction column after being precooled, the solution C enters another stainless steel reaction column after being precooled, the solution D enters a quenching kettle, ethyl acetate is added for purification after phase separation and concentration, and 2730g of oily 4-methoxy-benzaldehyde is obtained after concentration, and the yield is 75%. The capacity of the reaction device was 48 kg/day.
In conclusion, the jacketed type temperature-controllable continuous total-mixing stirring reactor provided by the invention has the advantages of high practicability and wide application range, can meet the requirements of most metallized organic reactions at-80-100 ℃, can ensure stable amplification of the reactions, and can prevent the problem of device blockage caused by side reaction products, so that the industrial amplified production process is stable, safe and controllable, and has higher yield.
In summary, the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, but any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (12)
1. The utility model provides a jacket formula controllable temperature continuous full mixing stirring reactor, its characterized in that includes shell, reation kettle suit, circulation oil bath seal groove and temperature control system, circulation oil bath seal groove fixed mounting is in the inside of shell, just circulation oil bath seal groove with temperature control system electric connection, reation kettle suit detachably installs in the inside of circulation oil bath seal groove, reation kettle suit includes a plurality of reation kettle that establish ties through the transfer pipeline.
2. The jacketed temperature-controllable continuous full-mixing stirring reactor according to claim 1, wherein the circulating oil bath seal groove comprises a detachable upper cover, and the reaction kettle sleeve is fixedly connected with the upper cover through a flange.
3. The jacketed, temperature-controllable, continuous, total-mixing, stirred reactor of claim 1, wherein the reaction kettle set comprises at least four reaction kettles, the reaction kettles having a volume of no more than 1000mL.
4. The jacketed, temperature-controllable, continuous, total-mixing, stirred reactor of claim 1, wherein the reactor set comprises 1 reactor with a volume of no more than 1000mL and 8 reactors with a volume of no more than 250 mL.
5. The jacketed type temperature-controllable continuous full-mixing stirring reactor according to claim 1, wherein a plurality of reaction columns and 1 thermocouple are arranged in each reaction kettle, and the reaction columns and the thermocouples are fixedly arranged in the reaction kettles through upper covers of the reaction kettles.
6. The jacketed type temperature-controllable continuous full-mixing stirring reactor according to claim 1, wherein the material of the reaction kettle is one selected from stainless steel, hastelloy or glass.
7. The jacketed temperature-controllable continuous full-mixing stirring reactor according to claim 1, wherein the reaction kettle is a magnetic stirring reaction kettle or a mechanical stirring reaction kettle.
8. The jacketed temperature-controllable continuous mixing reactor according to claim 1, wherein the transfer tube is made of stainless steel, hastelloy or soluble polytetrafluoroethylene PFA.
9. The jacketed temperature-controllable continuous full-mixing stirred reactor according to claim 1, wherein the pressure-resistant bearing ranges of the reaction kettle and the circulating oil bath seal groove are at least 10bar.
10. The jacketed temperature-controllable continuous full-mixing stirred reactor according to claim 1, wherein the reaction vessel and the transfer conduit are immersed in the medium of the circulating oil bath seal tank.
11. The jacketed temperature-controllable continuous full-mixing stirring reactor according to claim 1, wherein inert gas is introduced into the reaction kettle sleeve group, and the inert gas is used for providing driving force for a reaction system.
12. The jacketed, temperature-controllable, continuous, total-mixing, stirred reactor of claim 11, wherein the inert gas comprises nitrogen or argon.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211692162.7A CN116173867A (en) | 2022-12-28 | 2022-12-28 | Jacket type temperature-controllable continuous full-mixing stirring reactor |
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| CN202211692162.7A CN116173867A (en) | 2022-12-28 | 2022-12-28 | Jacket type temperature-controllable continuous full-mixing stirring reactor |
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