CN112961195A - Preparation method of ferrocenecarboxylic acid - Google Patents
Preparation method of ferrocenecarboxylic acid Download PDFInfo
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- CN112961195A CN112961195A CN202110284399.0A CN202110284399A CN112961195A CN 112961195 A CN112961195 A CN 112961195A CN 202110284399 A CN202110284399 A CN 202110284399A CN 112961195 A CN112961195 A CN 112961195A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
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- C07F17/00—Metallocenes
- C07F17/02—Metallocenes of metals of Groups 8, 9 or 10 of the Periodic System
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/05—Stirrers
- B01F27/051—Stirrers characterised by their elements, materials or mechanical properties
- B01F27/054—Deformable stirrers, e.g. deformed by a centrifugal force applied during operation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/83—Mixing plants specially adapted for mixing in combination with disintegrating operations
- B01F33/8305—Devices with one shaft, provided with mixing and milling tools, e.g. using balls or rollers as working tools; Devices with two or more tools rotating about the same axis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
- B01F33/8361—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating
- B01F33/83612—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating by crushing or breaking
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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
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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
- B01J19/0066—Stirrers
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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
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Abstract
The invention discloses a preparation method of ferrocenecarboxylic acid, which comprises the following steps: 1) a charging process; 2) a synthesis process; 3) a hydrolysis procedure: adding a part of crushed ice and deionized water into the hydrolysis kettle, carefully transferring the reaction mixed solution into the hydrolysis kettle, keeping the reaction mixed solution for 30-60 min, continuously adding the crushed ice while using nitrogen for isolation, keeping the temperature in the hydrolysis lower than 30 ℃, and continuously stirring for 2-3 hr to ensure complete hydrolysis; 4) filtering and washing; 5) and (5) a washing procedure. The invention isolates oxygen by introducing nitrogen in the hydrolysis procedure; and crushed ice is added in batches, the temperature of the hydrolysis kettle is continuously controlled, the materials are prevented from being oxidized before hydrolysis, and the generation of impurities is reduced.
Description
Technical Field
The invention relates to the field of production of ferrocenecarboxylic acid, and particularly relates to a preparation method of ferrocenecarboxylic acid.
Background
Currently, Ferrocene (Ferrocene) is a unique sandwich structure compound, and divalent iron ions are sandwiched between two planar rings and are in a staggered configuration. Ferrocene and its derivatives have their own characteristics: (1) aromaticity, can generate substitution reaction and is easy to modify; (2) lipophilic, capable of interacting with various enzymes inside the cell through the cell membrane; (3) low toxicity and can be metabolized in vivo. The ferrocene derivatives show wide pharmacological activity in the medical field, and particularly have outstanding pharmacological activity in the anti-tumor field: rosenefeld et al showed that ferrocene-modified cisplatin derivatives have considerable leukemia inhibitory activity and much lower nephrotoxicity than cis-DDP (A. Rosenfeld, et al. Inorg. Chim. Acat.1992,201: 219); studies by E.W.Neuse et al show that ferrocene derivatives have unique antitumor and anticancer activities (E.W.Neuse.J.Inorga.organic.polymers and materials.2005,15(1): 3-32); a series of ferrocene derivatives containing pyrazole rings are synthesized by X.F.Huang and the like, and activity studies show that part of the compounds have stronger anticancer activity than 5-fluorouracil (X.F.Huang, et al.J.Organomet.chem.2012,706-707: 113-123); liu et al synthesized a series of ferrocenyl urea derivatives, activity studies showed that some compounds had stronger inhibition of HIV-1 protease activity (W.Liu, et al, appl.organomet.chem.2012,26: 189-193); U.S. patent application 8426462B2 discloses that aromatic ring-containing ferrocene derivatives have strong inhibitory activity against human breast cancer cell line MDA-MB-231 and prostate cancer cell line PC-3. Ferrocenecarboxylic acid is an important intermediate of ferrocene and derivatives thereof.
The existing preparation method of ferrocenecarboxylic acid has the defect that materials are easily oxidized in the hydrolysis process.
Disclosure of Invention
The invention provides a preparation method of ferrocenecarboxylic acid aiming at the problems, and solves the defect that reactants are easily oxidized in the existing hydrolysis process of preparing ferrocenecarboxylic acid.
The technical scheme adopted by the invention is as follows:
a preparation method of ferrocenecarboxylic acid comprises the following steps:
1) a charging process: sequentially adding methylbenzene into a reaction kettle, starting stirring, adding ferrocene and methylbenzene, vacuumizing, continuously stirring, introducing cooling water to adjust the internal temperature to 15-18 ℃, and introducing carbon dioxide gas for 30-40 min;
2) a synthesis procedure: adding anhydrous AlCl into the reaction kettle3Continuously introducing carbon dioxide gas, keeping the internal temperature at 21-23 ℃, and keeping the temperature for 6-8 hr;
3) a hydrolysis procedure: adding a part of crushed ice and deionized water into the hydrolysis kettle, carefully transferring the reaction mixed solution into the hydrolysis kettle, keeping the reaction mixed solution for 30-60 min, continuously adding the crushed ice while using nitrogen for isolation, keeping the temperature in the hydrolysis lower than 30 ℃, and continuously stirring for 2-3 hr to ensure complete hydrolysis;
4) filtering and washing: centrifuging the hydrolyzed mixture with a centrifuge, washing the filter cake with deionized water to pH 6, air drying the filter cake, oven drying at 90-100 deg.C for 6-8hr, and pulverizing the solid with a crusher;
5) a washing procedure: pouring the crushed solid into a washing kettle filled with a mixed solution of toluene and deionized water, and fully stirring for 2-3 hr. The invention isolates oxygen by introducing nitrogen in the hydrolysis procedure; crushed ice is added in batches, the temperature of the hydrolysis kettle is continuously controlled, the materials are prevented from being oxidized before hydrolysis, and the generation of impurities is reduced; the problem that when crushed ice is put into the hydrolysis kettle for one time and the outside temperature is high, the crushed ice is melted too fast and the temperature of the hydrolysis kettle cannot be controlled continuously is avoided.
Optionally, the preparation method of ferrocenecarboxylic acid further comprises a filtering and re-washing process, wherein the filtering and re-washing process is to filter the mixed solution of the washing process by using a centrifuge, wash the mixed solution by 4-5 batches, wash each batch by using deionized water for 3-4 times until the mixed solution is neutral, and wash the mixed solution by using toluene for 3-4 times;
optionally, the preparation method of ferrocenecarboxylic acid further comprises the working procedures of filtering and washing again, wherein the drying working procedure is to naturally air-dry the filter cake in the working procedures of filtering and washing again, dry the filter cake at 103-105 ℃ for 4-6 hr, then crush the filter cake by a crusher, and dry the filter cake at 103-105 ℃ for 4-6 hr.
Optionally, the hydrolysis kettle comprises a kettle body, a hollow stirring rod is arranged in the kettle body, a first stirring blade is arranged in the middle of the stirring rod, a hollow cross rod is arranged at the bottom of the stirring rod, and crushed ice is thrown on the cross rod; a first driving motor is arranged in the center of the cross rod, a pair of transversely arranged stirring rollers is respectively arranged on the left side and the right side of the driving motor, first spiral blades are arranged on the stirring rollers, and the first spiral blades on the two sides are configured to drive crushed ice to move outwards when rotating; the hydrolysis kettle is worn out at the top of the stirring rod, a second driving motor is installed on one side of the top of the stirring rod, a first driven wheel is installed on the stirring rod, a first driving wheel is installed on the second driving motor, the first driving wheel is connected with a first driven wheel through belt transmission, a ventilating pipe used for introducing carbon dioxide is inserted downwards into the stirring rod from the top, a third driving motor is installed on the top of the stirring rod, a second driven wheel is installed on the ventilating pipe, a second driving wheel is installed on the second driving motor, the second driving wheel is connected with a second driven wheel through belt transmission, an ice throwing pipe which is obliquely arranged is installed on one side of the stirring rod, an annular charging tray is installed on the top of the ice throwing pipe, and the rotating speed of the ventilating pipe is greater than that of the stirring rod.
Optionally, the air pipe is provided with a guide vane on the inner area of the stirring rod, and the guide vane is configured to guide the air flow to flow downwards; the utility model discloses a crushing blade, including drainage blade, crushing blade, the lower supplementary section of multiunit spiral, drainage blade is connected to supplementary section top, and crushing blade is connected to the bottom, crushing blade is equipped with to the bottom of crushing blade, second helical blade is used for driving the crushed ice and moves down between drainage blade and the crushing blade, the breather pipe is through the external air supply of trade-over joint.
Optionally, a discharging stirring hopper is installed at the lower part of the outer side of the cross rod, the bottom of the discharging stirring hopper is a smooth S-shaped curved surface, an opening of the discharging stirring hopper faces outwards, a V-shaped cover plate is installed at the tail end of the cross rod, and the cover plate is used for unfolding outwards under the action of centrifugal force.
Optionally, the side wall of the blanking stirring hopper is provided with a filtering hole.
And a reset spring is arranged at the joint of the cover plate and the cross rod and used for driving the cover plate to seal an opening of the blanking stirring hopper.
Optionally, the side wall of the vent pipe is provided with a vent hole.
Due to the adoption of the technical scheme, the invention has the remarkable technical effects that:
1. the preparation method of the ferrocenecarboxylic acid comprises the steps of introducing nitrogen in a hydrolysis procedure to isolate oxygen; crushed ice is added in batches, the temperature of the hydrolysis kettle is continuously controlled, the materials are prevented from being oxidized before hydrolysis, and the generation of impurities is reduced; the problem that when crushed ice is put into the hydrolysis kettle for one time and the outside temperature is high, the crushed ice is melted too fast and the temperature of the hydrolysis kettle cannot be controlled continuously is avoided.
2. The feeding device is thrown into an ice feeding pipe through a charging disc, crushed ice enters a stirring rod and falls into a cross rod, a first driving motor drives a first helical blade to drive the crushed ice to be output outwards, the crushed ice flows downwards through an opening of a discharging stirring hopper, part of the crushed ice is filtered out through a filtering hole in the process, and larger crushed ice is unfolded or turned outwards under the action of centrifugal force of a cover plate along with the rotation of the cross rod and can be fed at a feeding speed by adjusting the rotating speed so as to enable the crushed ice to fall; meanwhile, the blanking stirring hopper rotates to stir materials to further drive the bottom materials to be mixed; crushed ice is thrown through the stirring rod instead of feeding through a feeding port, and continuous feeding and sealing feeding are effectively achieved.
3. According to the invention, the air flow is guided to flow downwards by rotating the vent pipe, so that the liquid is reduced from flowing backwards into the cross rod, meanwhile, the rotation of the crushing blade is used for crushing ice blocks to form fragments with smaller particle size, and meanwhile, the second spiral blade is rotated to drive the crushed ice to move downwards, so that the feeding efficiency is improved; the auxiliary slice further cuts and stirs the ice blocks on the crushing blade in the rotating process, and excessive materials are prevented from accumulating at the feeding port.
Description of the drawings:
FIG. 1 is a sectional view of a hydrolysis tank in the method for producing ferrocenecarboxylic acid according to example 3 of the present invention.
FIG. 2 is an enlarged view of part A of FIG. 1 of a hydrolysis reactor in the method for preparing ferrocenecarboxylic acid according to example 3 of the present invention.
FIG. 3 is a front view of a cover plate of a hydrolysis tank in the method for preparing ferrocenecarboxylic acid according to example 3 of the present invention.
FIG. 4 is a partial enlarged view of part B in FIG. 1 of a hydrolysis reactor in the method for preparing ferrocenecarboxylic acid according to example 3 of the present invention.
The figures are numbered:
1. the stirring device comprises a kettle body, 2, a stirring rod, 3, a first stirring blade, 4, a cross rod, 5, a first driving motor, 6, a stirring roller, 7, a first helical blade, 8, a second driving motor, 9, a first driven wheel, 10, a first driving wheel, 11, a vent pipe, 12, a third driving motor, 13, a second driven wheel, 14, a second driving wheel, 15, a charging tray, 16, a discharging stirring hopper, 17, a filtering hole, 18, a vent hole, 19, a drainage blade, 20, a crushing blade, 21, an auxiliary slice, 22, a second helical blade, 23, an ice feeding pipe, 24, a cover plate, 25 and a changing joint.
The specific implementation mode is as follows:
the present invention will be described in detail below with reference to the accompanying drawings.
In the present specification, the numerical range represented by "to" means a range in which the numerical values before and after "to" are included as the minimum value and the maximum value, respectively.
In the present specification, the term "step" is not limited to an independent step, and is included in the term as long as the intended purpose of the step is achieved even when the step cannot be clearly distinguished from other steps.
The percentage of the invention is mass percentage.
The reaction formula of the invention is as follows:
example 1
A preparation method of ferrocenecarboxylic acid comprises the following steps:
1) a charging process: adding toluene into a reaction kettle one by one, starting stirring, adding ferrocene and toluene, vacuumizing, continuously stirring, introducing cooling water to adjust the internal temperature to 15 ℃, and introducing carbon dioxide gas for 30 min;
2) a synthesis procedure: adding anhydrous AlCl into the reaction kettle3Continuously introducing carbon dioxide gas, maintaining the internal temperature at 21 deg.C, and maintaining for 6 hr;
3) a hydrolysis procedure: adding a part of crushed ice and deionized water into the hydrolysis kettle, carefully transferring the reaction mixture into the hydrolysis kettle, keeping the temperature in the hydrolysis kettle below 30 deg.C, continuously adding crushed ice for 2hr to ensure complete hydrolysis, wherein the reaction mixture is isolated with nitrogen gas for 30 min;
4) filtering and washing: centrifuging the hydrolyzed mixture by a centrifuge, washing the filter cake with deionized water to pH 6, naturally drying the filter cake, oven drying at 90 deg.C for 6hr, and pulverizing the solid with a crusher;
5) a washing procedure: pouring the pulverized solid into a washing kettle containing mixed solution of toluene and deionized water, and stirring thoroughly for 2 hr.
6) Filtration and rewashing steps: filtering the mixed solution in the washing procedure by using a centrifugal machine, washing by 4-5 batches, washing 3 times by using deionized water for each batch until the mixed solution is neutral, and washing 3 times by using toluene;
7) filtration and rewashing steps: naturally drying the filter cake after filtration and secondary washing, oven drying at 103 deg.C for 4hr, pulverizing with a crusher, and oven drying at 103 deg.C for 4 hr.
Example 2
A preparation method of ferrocenecarboxylic acid comprises the following steps:
1) a charging process: adding toluene into a reaction kettle one by one, starting stirring, adding ferrocene and toluene, vacuumizing, continuously stirring, introducing cooling water to adjust the internal temperature to 18 ℃, and introducing carbon dioxide gas for 40 min;
2) a synthesis procedure: adding anhydrous AlCl into the reaction kettle3Continuously introducing carbon dioxide gas, maintaining the internal temperature at 23 deg.C, and maintaining for 8 hr;
3) a hydrolysis procedure: adding a part of crushed ice and deionized water into the hydrolysis kettle, carefully transferring the reaction mixture into the hydrolysis kettle, keeping the temperature in the hydrolysis kettle below 30 deg.C for 3hr while keeping the temperature of crushed ice under nitrogen isolation for 60 min;
4) filtering and washing: centrifuging the hydrolyzed mixture with centrifuge, washing the filter cake with deionized water to pH 6, air drying the filter cake, oven drying at 90-100 deg.C for 8hr, and pulverizing the solid with crusher;
5) a washing procedure: pouring the pulverized solid into a washing kettle containing mixed solution of toluene and deionized water, and stirring thoroughly for 3 hr.
6) Filtration and rewashing steps: filtering the mixed solution in the washing procedure by using a centrifugal machine, washing by 4-5 batches, washing each batch by using deionized water for 4 times until the mixture is neutral, and washing by using toluene for 4 times;
7) filtration and rewashing steps: naturally drying the filter cake after filtration and secondary washing, oven drying at 105 deg.C for 6hr, pulverizing with a crusher, and oven drying at 105 deg.C for 6 hr.
Example 3
As shown in fig. 1, 2 and 3, the hydrolysis kettle of the invention comprises a kettle body 1, a hollow stirring rod 2 is arranged in the kettle body, a first stirring blade 3 is arranged in the middle of the stirring rod, a hollow cross rod 4 is arranged at the bottom of the stirring rod, and crushed ice is thrown on the cross rod; a first driving motor 5 is arranged in the center of the cross rod, a pair of transversely arranged stirring rollers 6 is respectively arranged on the left side and the right side of the driving motor, a first helical blade 7 is arranged on each stirring roller, and the first helical blades on the two sides are configured to drive crushed ice to move outwards when rotating; the hydrolysis kettle is worn out to the puddler top, second driving motor 8 is equipped with to the top one side of puddler, be equipped with on the puddler first from driving wheel 9, first action wheel 10 is equipped with on the second driving motor, first action wheel passes through belt drive and connects first from the driving wheel, the puddler has the breather pipe 11 that is used for letting in carbon dioxide by the top downwardly inserting, third driving motor 12 is equipped with at the top of puddler, it follows driving wheel 13 to be equipped with the second on the breather pipe, second action wheel 14 is equipped with on the second driving motor, the second action wheel passes through belt drive and connects the second from the driving wheel, the ice pipe 23 of throwing that the slope set up is equipped with to puddler one side, throw the ice pipe top and be equipped with annular charging tray 15. The breather pipe is externally connected with an external air source through a joint 25. The rotating speed of the breather pipe is greater than that of the stirring rod.
The lower part of the outer side of the cross rod is provided with a blanking stirring hopper 16, the bottom of the blanking stirring hopper is a smooth S-shaped curved surface, the opening of the blanking stirring hopper faces outwards, the tail end of the cross rod is provided with a V-shaped cover plate 24, and the cover plate is used for unfolding outwards under the action of centrifugal force. And the side wall of the blanking stirring hopper is provided with a filtering hole 17. And a reset spring is arranged at the joint of the cover plate and the cross rod and used for driving the cover plate to seal an opening of the blanking stirring hopper. The side wall of the vent pipe is provided with a vent hole 18.
In the implementation of the embodiment, crushed ice is thrown into the ice feeding pipe through the charging tray, enters the stirring rod and falls into the cross rod, the first spiral blade is driven by the first driving motor, the crushed ice is further driven to be output outwards, the crushed ice flows downwards through the opening of the discharging stirring hopper, part of the crushed ice is filtered out through the filtering holes in the process, the larger crushed ice is outwards unfolded or turned out under the action of the centrifugal force of the cover plate along with the rotation of the cross rod, and the feeding speed can be adjusted by adjusting the rotating speed, so that the crushed ice falls; meanwhile, the blanking stirring hopper rotates to stir materials to further drive the bottom materials to be mixed.
Example 4
As shown in fig. 4, the difference between the present embodiment 4 and the embodiment 3 is that the air pipe is provided with a guide vane 19 on the inner area of the stirring rod, and the guide vane is configured to guide the air flow to flow downwards; crushing blade 20 is equipped with to the below of drainage blade, crushing blade is used for smashing the ice-cube, be equipped with multiunit spiral between drainage blade and the crushing blade and assist section 21 downwards, drainage blade is connected at supplementary section top, and crushing blade is connected to the bottom, second helical blade 22 is equipped with to the bottom of crushing blade, second helical blade is used for driving the crushed ice and moves down.
When the embodiment is implemented, the air flow is driven and guided to flow downwards by rotating the vent pipe, so that the liquid is reduced from flowing backwards into the cross rod, meanwhile, the rotation of the crushing blade is used for crushing ice blocks to form fragments with smaller particle size, and meanwhile, the second spiral blade is rotated to drive the crushed ice to move downwards, so that the feeding efficiency is improved; the auxiliary slice further cuts and stirs the ice blocks on the crushing blade in the rotating process, and excessive materials are prevented from accumulating at the feeding port.
The above description is only for the preferred embodiment of the present invention and is not intended to limit the scope of the present invention, and all equivalent structural changes made by using the contents of the present specification and the drawings can be directly or indirectly applied to other related technical fields and are included in the scope of the present invention.
Claims (9)
1. A preparation method of ferrocenecarboxylic acid is characterized by comprising the following steps:
1) a charging process: sequentially adding methylbenzene into a reaction kettle, starting stirring, adding ferrocene and methylbenzene, vacuumizing, continuously stirring, introducing cooling water to adjust the internal temperature to 15-18 ℃, and introducing carbon dioxide gas for 30-40 min;
2) a synthesis procedure: adding anhydrous AlCl into the reaction kettle3Continuously introducing carbon dioxide gas, keeping the internal temperature at 21-23 ℃, and keeping the temperature for 6-8 hr;
3) a hydrolysis procedure: adding a part of crushed ice and deionized water into the hydrolysis kettle, carefully transferring the reaction mixed solution into the hydrolysis kettle, keeping the reaction mixed solution for 30-60 min, continuously adding the crushed ice while using nitrogen for isolation, keeping the temperature in the hydrolysis lower than 30 ℃, and continuously stirring for 2-3 hr to ensure complete hydrolysis;
4) filtering and washing: centrifuging the hydrolyzed mixture with a centrifuge, washing the filter cake with deionized water to pH 6, air drying the filter cake, oven drying at 90-100 deg.C for 6-8hr, and pulverizing the solid with a crusher;
5) a washing procedure: pouring the crushed solid into a washing kettle filled with a mixed solution of toluene and deionized water, and fully stirring for 2-3 hr.
2. The method for preparing ferrocenecarboxylic acid according to claim 1, further comprising a filtration and rewashing step of filtering the mixture obtained in the washing step with a centrifuge, washing the mixture in 4 to 5 batches, washing the mixture with deionized water 3 to 4 times per batch until the mixture becomes neutral, and washing the mixture with toluene 3 to 4 times.
3. The method for preparing ferrocenecarboxylic acid according to claim 2, further comprising a filtering and rewashing step, wherein the drying step comprises drying the filter cake obtained by the filtering and rewashing step naturally, drying the filter cake at 103 to 105 ℃ for 4 to 6hr, pulverizing the dried filter cake with a crusher, and drying the pulverized filter cake at 103 to 105 ℃ for 4 to 6 hr.
4. The method for preparing ferrocenecarboxylic acid according to claim 1, 2 or 3, wherein the hydrolysis kettle comprises a kettle body, a hollow stirring rod is arranged in the kettle body, a first stirring blade is arranged in the middle of the stirring rod, a hollow cross rod is arranged at the bottom of the stirring rod, and crushed ice is thrown on the cross rod; a first driving motor is arranged in the center of the cross rod, a pair of transversely arranged stirring rollers is respectively arranged on the left side and the right side of the driving motor, first spiral blades are arranged on the stirring rollers, and the first spiral blades on the two sides are configured to drive crushed ice to move outwards when rotating; the hydrolysis kettle is worn out at the top of the stirring rod, a second driving motor is installed on one side of the top of the stirring rod, a first driven wheel is installed on the stirring rod, a first driving wheel is installed on the second driving motor, the first driving wheel is connected with a first driven wheel through belt transmission, a ventilating pipe used for introducing carbon dioxide is inserted downwards into the stirring rod from the top, a third driving motor is installed on the top of the stirring rod, a second driven wheel is installed on the ventilating pipe, a second driving wheel is installed on the second driving motor, the second driving wheel is connected with a second driven wheel through belt transmission, an ice throwing pipe which is obliquely arranged is installed on one side of the stirring rod, an annular charging tray is installed on the top of the ice throwing pipe, and the rotating speed of the ventilating pipe is greater than that of the stirring rod.
5. The method for preparing ferrocenecarboxylic acid according to claim 4, wherein the air duct is provided with a guide blade on the area inside the stirring rod, and the guide blade is configured to guide the air flow to flow downwards; the utility model discloses a crushing blade, including drainage blade, crushing blade, the lower supplementary section of multiunit spiral, drainage blade is connected to supplementary section top, and crushing blade is connected to the bottom, crushing blade is equipped with to the bottom of crushing blade, second helical blade is used for driving the crushed ice and moves down between drainage blade and the crushing blade, the breather pipe is through the external air supply of trade-over joint.
6. The method for preparing ferrocenecarboxylic acid according to claim 5, wherein a blanking stirring hopper is arranged at the lower part of the outer side of the cross bar, the bottom of the blanking stirring hopper is a smooth S-shaped curved surface, the opening of the blanking stirring hopper faces outwards, a V-shaped cover plate is arranged at the tail end of the cross bar, and the cover plate is used for expanding outwards under the action of centrifugal force.
7. The method for preparing ferrocenecarboxylic acid according to claim 6, wherein the side wall of the blanking stirring hopper is provided with filtering holes.
8. The method for preparing ferrocenecarboxylic acid according to claim 6, wherein a return spring is arranged at the joint of the cover plate and the cross rod for driving the cover plate to seal the opening of the blanking stirring hopper.
9. The method for preparing ferrocenecarboxylic acid according to claim 6, wherein the vent tube has a vent hole in a sidewall thereof.
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| CN113769672A (en) * | 2021-08-11 | 2021-12-10 | 山东奔月生物科技股份有限公司 | Hydrolysis reaction device for neotame production |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2005060282A (en) * | 2003-08-11 | 2005-03-10 | Sankyo Organic Chem Co Ltd | Method for producing ferrocene derivative |
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| CN113769672A (en) * | 2021-08-11 | 2021-12-10 | 山东奔月生物科技股份有限公司 | Hydrolysis reaction device for neotame production |
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