CN114618414A - Reaction kettle for purifying cyclohexenecarboxylic acid and purification method thereof - Google Patents
Reaction kettle for purifying cyclohexenecarboxylic acid and purification method thereof Download PDFInfo
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- CN114618414A CN114618414A CN202210426384.8A CN202210426384A CN114618414A CN 114618414 A CN114618414 A CN 114618414A CN 202210426384 A CN202210426384 A CN 202210426384A CN 114618414 A CN114618414 A CN 114618414A
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- stirring
- reaction furnace
- purifying
- cyclohexenecarboxylic acid
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- 238000000746 purification Methods 0.000 title claims abstract description 117
- NMEZJSDUZQOPFE-UHFFFAOYSA-N Cyclohex-1-enecarboxylic acid Chemical compound OC(=O)C1=CCCCC1 NMEZJSDUZQOPFE-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 97
- 239000000463 material Substances 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000005265 energy consumption Methods 0.000 claims abstract description 7
- 239000000945 filler Substances 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims description 32
- 239000012528 membrane Substances 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000110 cooling liquid Substances 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000005260 corrosion Methods 0.000 claims description 7
- 230000007797 corrosion Effects 0.000 claims description 7
- 239000000741 silica gel Substances 0.000 claims description 7
- 229910002027 silica gel Inorganic materials 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 239000002826 coolant Substances 0.000 claims description 4
- AHHKQEGTXVWSBX-UHFFFAOYSA-N cyclohexene formic acid Chemical compound C(=O)O.C(=O)O.C1=CCCCC1 AHHKQEGTXVWSBX-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 230000003204 osmotic effect Effects 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 2
- KPJKBTKGZNETDU-UHFFFAOYSA-N cyclohexene;formic acid Chemical compound OC=O.C1CCC=CC1 KPJKBTKGZNETDU-UHFFFAOYSA-N 0.000 claims 1
- 238000002156 mixing Methods 0.000 abstract description 10
- 238000001914 filtration Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 2
- 238000003466 welding Methods 0.000 description 7
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000012044 organic layer Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
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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
- B01J19/0053—Details of the reactor
-
- 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
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
-
- 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
-
- 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
- B01J19/1893—Membrane reactors
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
Abstract
The invention discloses a reaction kettle for purifying cyclohexenecarboxylic acid and a purification method thereof, relates to the technical field of chemical industry, and aims to solve the problem that the working energy consumption of a cyclohexenecarboxylic acid purification device is higher due to low utilization efficiency of purification and filtration energy sources in the purification reaction kettle in the prior art. The upper end of reaction furnace casing is provided with agitator motor, the inside of reaction furnace casing is provided with the (mixing) shaft, the outside of (mixing) shaft is provided with first stirring purification pole support, the below of first stirring purification pole support is provided with second stirring purification pole support, the lower extreme of reaction furnace casing is provided with the outer support all around, the lower extreme of reaction furnace casing is provided with row material pipe, the upper end both sides of reaction furnace casing are provided with inlet pipe, heating pipe respectively, one side below of inlet pipe is provided with the filler pipe, the inside of reaction furnace casing is provided with the guiding disk, the lower extreme of guiding disk is provided with porous sieve cover.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a reaction kettle for purifying cyclohexenecarboxylic acid and a purification method thereof.
Background
In conventional devices, as in application No.: 201911372043.1, respectively; the name is: s-3-cyclohexene carboxylic acid and a refining method thereof. The device comprises: mixing the S-3-cyclohexenecarboxylic acid crude product, R-a-phenylethylamine and ethyl acetate, stirring, refluxing and filtering to obtain S-3-cyclohexenecarboxylic acid-R-a-phenylethylamine salt, wherein the S-3-cyclohexenecarboxylic acid crude product is S-3-cyclohexenecarboxylic acid with ee value less than 97%; mixing the S-3-cyclohexenecarboxylic acid-R-a-phenethylamine salt with ethanol, crystallizing and filtering to obtain a recrystallized material; and mixing and stirring dichloromethane, water and the recrystallized material, separating liquid, collecting an organic layer, and distilling the organic layer to obtain the S-3-cyclohexenecarboxylic acid. The refining method of S-3-cyclohexenecarboxylic acid provided by the invention can enable the ee value of the prepared S-3-cyclohexenecarboxylic acid to reach more than 99%, and meanwhile, the resolving agent R-phenylethylamine is recycled, so that the cost is saved.
However, the purifying device for the cyclohexenecarboxylic acid has the problem that the working energy consumption of the purifying device for the cyclohexenecarboxylic acid is high because the utilization efficiency of purifying and filtering energy inside the purifying reaction kettle is not high; therefore, the existing requirements are not met, and a reaction kettle for purifying cyclohexene formic acid and a purification method thereof are provided.
Disclosure of Invention
The invention aims to provide a reaction kettle for purifying cyclohexenecarboxylic acid and a purification method thereof, and aims to solve the problem that the work energy consumption of a cyclohexenecarboxylic acid purification device is high due to low utilization efficiency of purification and filtration energy inside the purification reaction kettle in the existing cyclohexenecarboxylic acid purification device in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the utility model provides a reation kettle is used in purification of cyclohexene formic acid, includes the reaction furnace casing, the upper end of reaction furnace casing is provided with agitator motor, the inside of reaction furnace casing is provided with the (mixing) shaft, and the (mixing) shaft is connected with agitator motor transmission, the outside of (mixing) shaft is provided with first stirring purification pole support, and first stirring purification pole support and (mixing) shaft welded connection, the below of first stirring purification pole support is provided with second stirring purification pole support, and second stirring purification pole support and (mixing) shaft welded connection, the lower extreme of reaction furnace casing is provided with the outer support all around, and outer support and reaction furnace casing bolt fixed connection, the lower extreme of reaction furnace casing is provided with row material pipe, and arranges material pipe and reaction furnace casing welded connection, the upper end both sides of reaction furnace casing are provided with inlet pipe, heating pipe respectively, one side below of inlet pipe is provided with the filler pipe, the water feeding pipe is connected with a pipeline flange of the reaction furnace shell, the inside of the reaction furnace shell is provided with a flow guide plate, the flow guide plate is connected with the inner wall of the reaction furnace shell in a welding mode, the lower end of the flow guide plate is provided with a porous sieve cover, and the porous sieve cover and the flow guide plate are integrally formed.
Preferably, each purification pole's inside all is provided with the connecting axle, and the connecting axle respectively with first stirring purification pole support, second stirring purification pole support pivot connection, purification pole outer wall is provided with porous shell.
Preferably, the outside a week of connecting axle is provided with the purification board, and the inner wall welded connection of purification board and purification pole, every the inside of purification board all is provided with the cooling plate, the both sides of cooling plate all are provided with corrosion-resistant silica gel groove.
Preferably, each corrosion-resistant silica gel groove's the outside all is provided with one-way membrane of accomodating, and one-way membrane and the cooling plate card groove fixed connection of accomodating, the both sides of purification board all are provided with porous osmotic membrane.
Preferably, each of the cooling plates is provided with a cooling liquid therein.
Preferably, a soaking plate is arranged outside the cooling liquid, and the soaking plate is connected with the inner wall of the cooling plate in a welding mode.
Preferably, the lower ends of the first stirring purifying rod support and the second stirring purifying rod support are respectively provided with a purifying rod, and the purifying rods are connected with the first stirring purifying rod support and the second stirring purifying rod support in a rotating shaft manner.
Preferably, the lower end of the stirring shaft is provided with a connecting shaft bearing, the connecting shaft bearing is fixedly connected with the porous sieve cover bolt, and the connecting shaft bearing is connected with the stirring shaft bearing.
Preferably, the use method of the reaction kettle for purifying the cyclohexene carboxylic acid comprises the following steps:
the method comprises the following steps: the reaction furnace comprises a reaction furnace shell, a stirring motor, a stirring shaft, a first stirring purification rod support, a second stirring purification rod support, a heating pipe, a flow guide disc, a porous sieve cover and a connecting shaft, wherein materials are firstly put into the reaction furnace from a feeding pipe, then a water adding pipe is used for controlling the water amount, the stirring shaft is controlled by the stirring motor to rotate, the mixture is fully stirred, the purification rods at the lower ends of the first stirring purification rod support and the second stirring purification rod support fully stir the materials, the heating pipe is used for heating the materials, and the separation of the cyclohexene carboxylate is accelerated;
step two: when the cyclohexenecarboxylic acid is heated and stirred, the cyclohexenecarboxylic acid can pass through the porous shell of the purification rod and then is deposited on two sides of the interior of the purification plate, the surface area of the purification plate in contact with the cyclohexenecarboxylic acid is greatly increased, so that the cyclohexenecarboxylic acid can be attached to the purification plate at an accelerated speed to complete purification, the cyclohexenecarboxylic acid passes through the porous permeable membrane and is deposited on the unidirectional storage membrane, after the deposition is finished, the unidirectional storage membrane can be detached from the groove of the cooling plate, the unidirectional storage membrane can prevent the cyclohexenecarboxylic acid from overflowing, and the purification efficiency of the cyclohexenecarboxylic acid is greatly improved;
step three: the inside coolant liquid of cooling plate can absorb the heat of cooling plate fast for the cooling plate both sides form with the external environment between the temperature difference, cyclohexene carboxylic acid is one-way accomodate the membrane and is flowed to its inside with higher speed, cyclohexene carboxylic acid has greatly been improved and has been one-way accomodate the inside fixed of membrane, thereby realized the separation of purification with higher speed to cyclohexene carboxylic acid, current cyclohexene carboxylic acid purification device has been solved, because the inside purification of purification reation kettle filters energy utilization efficiency not high, cause the higher problem of cyclohexene carboxylic acid purification device work energy consumption.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, through the arrangement of the reaction furnace shell, the stirring motor, the stirring shaft, the first stirring purification rod support, the second stirring purification rod support, the heating pipe, the flow guide disc, the porous sieve cover and the connecting shaft, materials are firstly put in from the feeding pipe, then the feeding pipe controls the water quantity, the stirring motor controls the rotation of the stirring shaft, the mixture is fully stirred, the purification rods at the lower ends of the first stirring purification rod support and the second stirring purification rod support fully stir the materials, the heating pipe heats the materials, and the separation of the cyclohexene carboxylate is accelerated.
2. Through the setting of purification board, when cyclohexenecarboxylic acid is heated when stirring, cyclohexenecarboxylic acid can pass the porous shell of purification pole, later the deposit is in the inside both sides of purification board, the purification board has greatly improved the surface area with the contact of cyclohexenecarboxylic acid, make cyclohexenecarboxylic acid can accelerate to adhere to and accomplish the purification at the purification board, cyclohexenecarboxylic acid passes porous osmotic membrane deposit and accomodates the membrane in one-way, after the deposit, can accomodate the membrane in one-way and lift off from the recess of cooling plate, it is excessive that cyclohexenecarboxylic acid can prevent to accomodate the membrane in one-way, the purification efficiency to cyclohexenecarboxylic acid has greatly been improved.
3. Through the setting of cooling plate, the inside coolant liquid of cooling plate can fast absorb the heat of cooling plate, make the cooling plate both sides form and the external environment between the temperature difference, cyclohexene carboxylic acid flows to its inside at one-way membrane of accomodating with higher speed, cyclohexene carboxylic acid has greatly been improved and has been accomodate the inside fixed of membrane in one-way, thereby the separation of purification with higher speed to cyclohexene carboxylic acid has been realized, current cyclohexene carboxylic acid purification device has been solved, because the inside purification of purification reation kettle filters energy utilization efficiency not high, cause cyclohexene carboxylic acid purification device work energy consumption than higher problem.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a cross-sectional view of a refining rod according to the present invention;
FIG. 3 is a schematic view of the internal structure of the purification plate of the present invention;
FIG. 4 is a schematic view of the internal structure of the cooling plate of the present invention;
FIG. 5 is an enlarged view of a portion of the present invention at A;
in the figure: 1. a reactor housing; 2. a stirring motor; 3. a stirring shaft; 4. a first stir bar support; 5. a second stir bar support; 6. a purification rod; 7. a feeding pipe; 8. heating a tube; 9. a water feeding pipe; 10. an outer support; 11. a discharge pipe; 12. a flow guide disc; 13. a perforated screen cover; 14. a connecting shaft; 15. purifying the plate; 16. a porous shell; 17. a porous, permeable membrane; 18. a cooling plate; 19. a corrosion-resistant silica gel tank; 20. a one-way receiving film; 21. cooling liquid; 22. a vapor chamber; 23. and a connecting shaft bearing.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1-5, an embodiment of the present invention is shown: a reaction kettle for purifying cyclohexenecarboxylic acid comprises a reaction furnace shell 1, wherein a stirring motor 2 is arranged at the upper end of the reaction furnace shell 1, a stirring shaft 3 is arranged inside the reaction furnace shell 1, the stirring shaft 3 is in transmission connection with the stirring motor 2, a first stirring and purifying rod support 4 is arranged outside the stirring shaft 3, the first stirring and purifying rod support 4 is in welding connection with the stirring shaft 3, a second stirring and purifying rod support 5 is arranged below the first stirring and purifying rod support 4, the second stirring and purifying rod support 5 is in welding connection with the stirring shaft 3, an outer support 10 is arranged around the lower end of the reaction furnace shell 1, the outer support 10 is in bolt fixed connection with the reaction furnace shell 1, a material discharging pipe 11 is arranged at the lower end of the reaction furnace shell 1, the material discharging pipe 11 is in welding connection with the reaction furnace shell 1, and a material inlet pipe 7 is respectively arranged at two sides of the upper end of the reaction furnace shell 1, The reactor comprises a heating pipe 8, a water feeding pipe 9 is arranged below one side of a feeding pipe 7, the water feeding pipe 9 is connected with a pipeline flange of a reactor shell 1, a flow guide disc 12 is arranged inside the reactor shell 1, the flow guide disc 12 is connected with the inner wall of the reactor shell 1 in a welding mode, a porous sieve cover 13 is arranged at the lower end of the flow guide disc 12, and the porous sieve cover 13 and the flow guide disc 12 are integrally formed.
Further, a connecting shaft 14 is arranged inside each purification rod 6, the connecting shaft 14 is respectively connected with the first stirring purification rod bracket 4 and the second stirring purification rod bracket 5 in a rotating mode, and a porous shell 16 is arranged on the outer wall of each purification rod 6.
Further, purification board 15 is arranged on one circumference of the outer side of connecting shaft 14, purification board 15 is connected with the inner wall of purification rod 6 in a welding mode, cooling board 18 is arranged inside each purification board 15, and corrosion-resistant silica gel grooves 19 are arranged on two sides of each cooling board 18.
Further, the outer side of each corrosion-resistant silica gel groove 19 is provided with a one-way storage film 20, the one-way storage films 20 are fixedly connected with the clamping grooves of the cooling plates 18, and the two sides of the purification plate 15 are provided with porous permeable films 17.
Further, each cooling plate 18 is provided with a cooling liquid 21 inside.
Further, a soaking plate 22 is provided outside the cooling liquid 21, and the soaking plate 22 is welded to the cooling liquid 21.
Further, the lower ends of the first stirring and purifying rod support 4 and the second stirring and purifying rod support 5 are respectively provided with a purifying rod 6, and the purifying rod 6 is connected with the first stirring and purifying rod support 4 and the second stirring and purifying rod support 5 in a rotating shaft mode.
Further, the lower end of the stirring shaft 3 is provided with a connecting shaft bearing 23, the connecting shaft bearing 23 is fixedly connected with the porous sieve cover 13 through bolts, and the connecting shaft bearing 23 is connected with the stirring shaft 3 through bearings.
Further, a use method of the reaction kettle for purifying the cyclohexene carboxylic acid comprises the following steps:
the method comprises the following steps: the reaction furnace comprises a reaction furnace shell 1, a stirring motor 2, a stirring shaft 3, a first stirring purification rod support 4, a second stirring purification rod support 5, a heating pipe 8, a flow guide disc 12, a porous sieve cover 13 and a connecting shaft 14, wherein materials are firstly put into the reaction furnace from a feeding pipe 7, then a water adding pipe 9 is used for controlling the water amount, the stirring motor 2 is used for controlling the stirring shaft 3 to rotate, the mixture is fully stirred, the materials are fully stirred by purification rods 6 at the lower ends of the first stirring purification rod support 4 and the second stirring purification rod support 5, and the heating pipe 8 is used for heating the materials, so that the precipitation of cyclohexene carboxylic acid is accelerated;
step two: when the cyclohexenecarboxylic acid is heated and stirred, the cyclohexenecarboxylic acid passes through the porous shell 16 of the purifying rod 6 and then is deposited on two sides of the interior of the purifying plate 15, the surface area of the purifying plate 15 in contact with the cyclohexenecarboxylic acid is greatly increased, so that the cyclohexenecarboxylic acid can be attached to the purifying plate 15 at an accelerated speed to complete purification, the cyclohexenecarboxylic acid passes through the porous permeable membrane 17 and is deposited on the unidirectional storage membrane 20, after the deposition is finished, the unidirectional storage membrane 20 can be detached from the groove of the cooling plate 18, the unidirectional storage membrane 20 can prevent the cyclohexenecarboxylic acid from overflowing, and the purifying efficiency of the cyclohexenecarboxylic acid is greatly improved;
step three: the inside coolant liquid 21 of cooling plate 18 can absorb the heat of cooling plate 18 fast, make cooling plate 18 both sides form and the external environment between the temperature difference, cyclohexene carboxylic acid is being one-way accomodate membrane 20 and is flowing to its inside with higher speed, cyclohexene carboxylic acid has greatly been improved and has been one-way accomodate the inside fixed of membrane 20, thereby the separation of purification with higher speed to cyclohexene carboxylic acid has been realized, current cyclohexene carboxylic acid purification device has been solved, because the inside purification of purification reation kettle filters energy utilization efficiency not high, cause the higher problem of cyclohexene carboxylic acid purification device work energy consumption.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (9)
1. The utility model provides a cyclohexene formic acid purifies uses reation kettle, includes reaction furnace housing (1), its characterized in that: the reaction furnace comprises a reaction furnace shell (1), wherein a stirring motor (2) is arranged at the upper end of the reaction furnace shell (1), a stirring shaft (3) is arranged inside the reaction furnace shell (1), the stirring shaft (3) is in transmission connection with the stirring motor (2), a first stirring purification rod support (4) is arranged outside the stirring shaft (3), the first stirring purification rod support (4) is in welded connection with the stirring shaft (3), a second stirring purification rod support (5) is arranged below the first stirring purification rod support (4), the second stirring purification rod support (5) is in welded connection with the stirring shaft (3), an outer support (10) is arranged around the lower end of the reaction furnace shell (1), the outer support (10) is in bolt fixed connection with the reaction furnace shell (1), a discharge pipe (11) is arranged at the lower end of the reaction furnace shell (1), and the discharge pipe (11) is in welded connection with the reaction furnace shell (1), the utility model discloses a reactor, including reaction furnace shell (1), inlet pipe (7), heating pipe (8) are provided with respectively to the upper end both sides of reaction furnace shell (1), one side below of inlet pipe (7) is provided with filler pipe (9), and filler pipe (9) and reaction furnace shell (1) pipe flange joint, the inside of reaction furnace shell (1) is provided with flow guide disc (12), and flow guide disc (12) and the inner wall welded connection of reaction furnace shell (1), the lower extreme of flow guide disc (12) is provided with porous sieve cover (13), and porous sieve cover (13) and flow guide disc (12) integrated into one piece setting.
2. The reaction kettle for purifying cyclohexenecarboxylic acid as claimed in claim 1, wherein: every purification pole (6) inside all is provided with connecting axle (14), and connecting axle (14) respectively with first stirring purification pole support (4), second stirring purification pole support (5) pivot connection, purification pole (6) outer wall is provided with porous shell (16).
3. The reaction kettle for purifying cyclohexenecarboxylic acid as claimed in claim 2, wherein: purification board (15) are provided with in outside a week of connecting axle (14), and purification board (15) and the inner wall welded connection of purification pole (6), every the inside of purification board (15) all is provided with cooling plate (18), the both sides of cooling plate (18) all are provided with corrosion-resistant silica gel groove (19).
4. The reaction kettle for purifying cyclohexenecarboxylic acid as claimed in claim 3, wherein: every the outside in corrosion-resistant silica gel groove (19) all is provided with one-way membrane (20) of accomodating, and one-way membrane (20) of accomodating and cooling plate (18) draw-in groove fixed connection, the both sides of purification board (15) all are provided with porous osmotic membrane (17).
5. The reaction kettle for purifying cyclohexenecarboxylic acid as claimed in claim 3, wherein: the interior of each cooling plate (18) is provided with a cooling liquid (21).
6. The reaction kettle for purifying cyclohexenecarboxylic acid as claimed in claim 5, wherein: and a soaking plate (22) is arranged outside the cooling liquid (21).
7. The reaction kettle for purifying cyclohexenecarboxylic acid as claimed in claim 1, wherein: purification pole (6) are all provided with to the lower extreme of first stirring purification pole support (4) and second stirring purification pole support (5), and purification pole (6) are connected with first stirring purification pole support (4), second stirring purification pole support (5) pivot.
8. The reaction kettle for purifying cyclohexenecarboxylic acid as claimed in claim 1, wherein: the lower end of the stirring shaft (3) is provided with a connecting shaft bearing (23), the connecting shaft bearing (23) is fixedly connected with the porous sieve cover (13) through bolts, and the connecting shaft bearing (23) is connected with the stirring shaft (3) through bearings.
9. The use method of the reaction kettle for purifying the cyclohexene formic acid as claimed in any one of claims 1 to 8, which is characterized by comprising the following steps:
the method comprises the following steps: the reaction furnace comprises a reaction furnace shell (1), a stirring motor (2), a stirring shaft (3), a first stirring purification rod support (4), a second stirring purification rod support (5), a heating pipe (8), a flow guide disc (12), a porous sieve cover (13) and a connecting shaft (14), wherein materials are firstly put into the reaction furnace from a feeding pipe (7), then a water adding pipe (9) controls the water amount to be put into the reaction furnace, the stirring motor (2) controls the stirring shaft (3) to rotate, the mixture is fully stirred, the materials are fully stirred by purification rods (6) at the lower ends of the first stirring purification rod support (4) and the second stirring purification rod support (5), the materials are heated by the heating pipe (8), and the precipitation of the cyclohexene formate is accelerated;
step two: when the cyclohexenecarboxylic acid is heated and stirred, the cyclohexenecarboxylic acid can pass through the porous shell (16) of the purifying rod (6) and then is deposited on two sides of the interior of the purifying plate (15), the surface area of the purifying plate (15) contacted with the cyclohexenecarboxylic acid is greatly improved, so that the cyclohexenecarboxylic acid can be attached to the purifying plate (15) at an accelerated speed to complete purification, the cyclohexenecarboxylic acid passes through the porous permeable membrane (17) and is deposited on the unidirectional storage membrane (20), after the deposition is finished, the unidirectional storage membrane (20) can be detached from the groove of the cooling plate (18), the unidirectional storage membrane (20) can prevent the cyclohexenecarboxylic acid from overflowing, and the purifying efficiency of the cyclohexenecarboxylic acid is greatly improved;
step three: inside coolant liquid (21) of cooling plate (18) can absorb the heat of cooling plate (18) fast, make cooling plate (18) both sides form and the external environment between the temperature difference, cyclohexene carboxylic acid is accomodate membrane (20) in one-way and is flowed to its inside with higher speed, cyclohexene carboxylic acid has greatly been improved and has been accomodate inside fixed of membrane (20) in one-way, thereby realized the separation of purification with higher speed to cyclohexene carboxylic acid, current cyclohexene carboxylic acid purification device has been solved, because the inside purification of purification reation kettle filters energy utilization efficiency not high, cause the higher problem of cyclohexene carboxylic acid purification device work energy consumption.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210426384.8A CN114618414B (en) | 2022-04-22 | 2022-04-22 | Reaction kettle for purifying cyclohexenecarboxylic acid and purification method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210426384.8A CN114618414B (en) | 2022-04-22 | 2022-04-22 | Reaction kettle for purifying cyclohexenecarboxylic acid and purification method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114618414A true CN114618414A (en) | 2022-06-14 |
| CN114618414B CN114618414B (en) | 2023-11-07 |
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| JP2000233105A (en) * | 1999-02-15 | 2000-08-29 | Michio Watanabe | Multistep type filtration apparatus |
| JP2004217473A (en) * | 2003-01-15 | 2004-08-05 | Sharp Corp | Apparatus and method for purifying silicon and silicon purified using the same |
| US20090149562A1 (en) * | 2004-09-13 | 2009-06-11 | Stefan Nordhoff | Purification of a distilled bottom product containing (meth)acrylic acid by means of a crystallization process |
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| CN113967441A (en) * | 2021-11-17 | 2022-01-25 | 连云港瑞邦药业有限公司 | Purification and filling device and method for calcium gluconate production |
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| CN114618414B (en) | 2023-11-07 |
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