CN114011370A - Equipment for efficiently producing pyrazolecarboxylic acid and improvement method thereof - Google Patents
Equipment for efficiently producing pyrazolecarboxylic acid and improvement method thereof Download PDFInfo
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- CN114011370A CN114011370A CN202210015168.4A CN202210015168A CN114011370A CN 114011370 A CN114011370 A CN 114011370A CN 202210015168 A CN202210015168 A CN 202210015168A CN 114011370 A CN114011370 A CN 114011370A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0003—Condensation of vapours; Recovering volatile solvents by condensation by using heat-exchange surfaces for indirect contact between gases or vapours and the cooling medium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/18—Absorbing units; Liquid distributors therefor
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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
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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
- 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
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D231/00—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings
- C07D231/02—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings
- C07D231/10—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D231/14—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
Abstract
The invention discloses equipment for efficiently producing pyrazole formic acid and an improvement method thereof, and the equipment comprises a preparation reaction kettle, wherein a tail gas collecting box and a heating box are arranged on the surface of the preparation reaction kettle, the heating box is positioned above the tail gas collecting box, a condenser and a pressure pump are arranged on the surface of the preparation reaction kettle, a heating interlayer is arranged inside the heating box, a heat conducting hose is arranged on the inner wall of the heating box in a penetrating manner, a second one-way valve is arranged inside the heat conducting hose, the tail end of the heat conducting hose extends back to the inside of the heating box, two groups of electronic control valves which are arranged at equal intervals are arranged on the surface of the heat conducting hose, a heat insulating sliding plate is arranged on the inner wall of the heating box, and electric telescopic rods are arranged at four corners of the top of the heat insulating sliding plate; and an electronic display screen is arranged on the surface of the heating box. By arranging the heating box and the condenser, the temperature rise and refrigeration of the inner tank in the same space can be effectively isolated and adjusted, so that the requirement of temperature change is met, and the yield is improved.
Description
Technical Field
The invention relates to the technical field of chemical substance synthesis, in particular to equipment for efficiently producing pyrazolecarboxylic acid and an improved method thereof.
Background
The 3-bromo-1- (3-chloropyridin-2-yl) -1H-pyrazole-5-formic acid is an important intermediate of the bisamide insecticide chlorantraniliprole, the chlorantraniliprole has a wide insecticidal object range, can be used for various crops, and has the advantages of good persistence, good activity, low toxicity, environmental biological safety, no cross resistance with mainstream insecticide products in the market, good miscibility with various bulk insecticides, and wide attention by the domestic and foreign pesticide markets.
The existing chemical substance synthesis preparation equipment has the defects that:
1. patent document CN102952007A discloses a single set of annual production apparatus for 10 ten thousand tons of formic acid, which comprises a carbonyl reactor, a methyl ester rectifying tower, a methyl ester storage tank, a first hydrolysis reactor, a second hydrolysis reactor, an acid tower, a diacid tower and a triacid tower, wherein the bottom outlet of the carbonyl reactor is connected with the middle inlet of the methyl ester rectifying tower, the top of the methyl ester rectifying tower is connected with the top of the condensed liquid methyl ester storage tank, the bottom outlet of the methyl ester storage tank is connected with the bottom of the first hydrolysis reactor, the upper outlet of the first hydrolysis reactor is connected with the lower inlet of the second hydrolysis reactor, the upper outlet of the second hydrolysis reactor is connected with the middle inlet of the acid tower, the bottom outlet of the acid tower is connected with the middle inlet of the diacid tower, the lower outlet of the diacid tower is connected with the middle inlet of the triacid tower, a carbon monoxide gas distributor is arranged in the carbonyl reactor, the first hydrolysis reactor, the second hydrolysis reactor, the third hydrolysis reactor and the third hydrolysis reactor, The second hydrolysis reactor is internally provided with heating. The device has safe and simple operation, reduces production links, reduces production cost, prolongs the service life of equipment, and improves economic benefit, and the heating temperature can not be effectively adjusted in the using process of the device;
2. patent document CN211436142U discloses a formic acid carbonyl reactor, "which comprises: the device comprises a tower body, an air inlet, an air distribution device, an air outlet valve, a sprayer, a liquid discharge pipe and an exhaust pipe; the tower body is of a closed structure with a cavity, the bottom of the tower body is provided with two air inlets, and the two air inlets are symmetrically arranged relative to the tower body; the gas distribution device is arranged in the tower body and consists of at least three circles of concentrically arranged distribution pipes, the diameters of the distribution pipes are sequentially reduced from outside to inside, the distribution pipes are communicated with the gas inlet, the gas outlet valve is arranged on the distribution pipes, the spray pipe is positioned above the gas outlet valve in the tower body, and the liquid discharge pipe is arranged at the bottom of the tower body; the exhaust pipe is arranged on the upper sealing cover of the tower body. The reactor designed by the application can realize the uniform distribution of CO in the carbonyl reactor, improve the mass transfer rate of gas-liquid two phases, increase the reaction rate and improve the yield of formic acid, and the device can not realize the classified collection and purification treatment of tail gas in the using process, so that the tail gas is directly discharged without effective treatment, the environment is influenced, and the recycling of effective components is not facilitated;
3. patent document CN211435137U discloses a rectification preparation device of high-concentration formic acid, "comprising: the rectifying tower is used for rectifying, and a feeding pipeline is arranged in the middle of the rectifying tower; a reboiler connected to the bottom of the rectifying tower; the inlet of the condenser is connected with the top of the rectifying tower; the inlet of the reflux tank is connected with the outlet of the condenser, and the outlet of the reflux tank is connected with the top of the rectifying tower through a reflux pump; and the inlet of the vacuum pump is connected with the outlet end of the condenser through a pipeline, and the outlet of the vacuum pump is connected with the washing tower. The device can conveniently and effectively prepare high-concentration formic acid through rectification, and the device cannot realize pressure adjustment and pressure relief treatment in the reaction process in the using process, so that the chemical combination reaction speed is low;
4. patent document CN211178054U discloses an internal formic acid circulation cooling system, "comprising a desalted water cooling system and a circulating water cooling system, wherein the desalted water cooling system comprises a desalted water storage tank, a desalted water pump and a cold medium channel of a desalted water heat exchanger which are connected in sequence, the hot medium channel of the desalted water heat exchanger is used for being connected with a gas-phase formic acid source, and the outlet of the cold medium channel of the desalted water heat exchanger is connected with the desalted water storage tank; the circulating water cooling system comprises a water cooling tower, a circulating water pump and a cold medium channel of the heat exchanger which are connected in sequence, and the outlet of the cold medium channel of the heat exchanger is connected with the water cooling tower; the heat medium channel of the heat exchanger is connected between the desalted water pump and the desalted water heat exchanger. The cooling system can better overcome the influence of scaling of heat exchange equipment and improve the heat exchange efficiency, and the device can not realize effective heat insulation treatment with a heating device in the use process, so that the refrigeration efficiency of the device is lower.
Disclosure of Invention
The present invention has been made to solve the above-mentioned problems occurring in the prior art, and an object of the present invention is to provide an apparatus for efficiently producing pyrazolecarboxylic acid and an improved method thereof.
In order to achieve the purpose, the invention provides the following technical scheme: the equipment for efficiently producing the pyrazole formic acid comprises a preparation reaction kettle, wherein a tail gas collecting box and a heating box are arranged on the surface of the preparation reaction kettle, the heating box is positioned above the tail gas collecting box, a condenser and a pressure pump are arranged on the surface of the preparation reaction kettle, the pressure pump is positioned below the condenser, and the tail gas collecting box is positioned on one side of the pressure pump;
the heating box is characterized in that a heating interlayer is arranged inside the heating box, a heat conduction hose penetrates through the inner wall of the heating box, a second one-way valve is arranged inside the heat conduction hose, the tail end of the heat conduction hose extends back to the inside of the heating box, two groups of electronic control valves which are arranged at equal intervals are arranged on the surface of the heat conduction hose, a heat insulation sliding plate is arranged on the inner wall of the heating box, and electric telescopic rods are arranged at four corners of the top of the heat insulation sliding plate;
and an electronic display screen is arranged on the surface of the heating box.
Preferably, the internally mounted of box is collected to tail gas has the cross baffle frame, the internal space of box is collected to tail gas divides into the first cavity of collecting of four independent spaces, second collection cavity, third collection cavity and fourth collection cavity through the cross baffle frame, and first collection cavity, second collection cavity, third collection cavity and fourth collection cavity anticlockwise arrange, the inside of cross baffle frame is run through and is installed the siphunculus, cavity and third collection cavity, first collection cavity and second collection cavity, third collection cavity and fourth collection cavity are all connected through the siphunculus, the internally mounted of siphunculus has parallel arrangement's ventilated membrane and first check valve.
3. The apparatus for efficiently producing pyrazolecarboxylic acid according to claim 1, wherein: the output of force (forcing) pump is connected with the air duct, the surface mounting of air duct has the outlet duct, and the tail end of outlet duct extends into the inside of fourth collection cavity, the surface mounting of outlet duct has the solenoid valve, the third check valve is all installed to the inside of outlet duct and air duct, the inside third check valve of air duct is located the place ahead of air duct and outlet duct junction, the tail end surface mounting of air duct has pressure sensors.
Preferably, the surface mounting of condenser has the air hose that supplies gas that the equidistance was arranged, the surface of air hose encircles and installs No. two insulation boards, the electro-magnet is installed to the inner wall of No. two insulation boards, No. two insulation board's inside slidable mounting has a insulation board, the width of an insulation board is less than No. two insulation boards, the end-to-end connection of an insulation board has the magnetic stripe, the width of magnetic stripe is the same with the width of No. two insulation boards, the surface mounting of No. two insulation boards has the electron thermometer, and electron thermometer and electronic display screen electric connection.
Preferably, the internally mounted of preparation reation kettle has the inner tank, and the tail end of air duct extends into the inside of inner tank, the space that inner tank and preparation reation kettle inner wall pressed from both sides becomes is the heat treatment intermediate layer, and heat conduction hose and air feed hose all are located the interbedded inside of heat treatment, the temperature-sensing ware is installed to the inner wall of inner tank, and temperature-sensing ware and electronic display screen electric connection.
Preferably, the seal cover is installed at the top of preparation reation kettle, first feed inlet, second feed inlet, third feed inlet and fourth feed inlet have been arranged to the top matrix of seal cover, first feed inlet and second feed inlet symmetrical arrangement, third feed inlet and fourth feed inlet symmetrical arrangement, the tail end of first feed inlet, second feed inlet, third feed inlet and fourth feed inlet all extends into the inside of inner tank.
Preferably, a driving motor is installed at the top of the sealing top cover, a stirring paddle is installed at the output end of the driving motor, and the stirring paddle is located inside the inner tank.
Preferably, the surface mounting of box is collected to tail gas has the row of arranging material pipe of matrix arrangement, and the tail end of four groups of row material pipes extends into the inside of first collection cavity, second collection cavity, third collection cavity and fourth collection cavity respectively, every group the surface of arranging the material pipe all installs the valve.
Preferably, the exhaust pipe is installed at the top of the tail gas collecting box, and the tail end of the exhaust pipe penetrates through the first collecting cavity and extends into the first collecting cavity.
Preferably, the working steps of the improved method are as follows:
s1, adding a solvent into the inner tank through the first feed port, immediately putting 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-ethyl formate into the inner tank through the second feed port, then adding a brominating agent through the third feed port to carry out bromination reaction, wherein the solvent is a mixture of dimethylformamide or dimethylacetamide and R-ClnBrm, R-is C1-C3 alkyl or phenyl, n and m are 0 or natural numbers of 1-8, the brominating agent is a mixture of bromine and an auxiliary brominating agent, and the auxiliary brominating agent is a mixture of bromine and an auxiliary brominating agent
(N-bromoamide),
One or more of (N-bromosuccinimide), phosphorus oxybromide, phosphorus tribromide and thionyl bromide;
s2, adding an oxidant into the S1 reaction liquid through a fourth feed inlet, starting a heating interlayer in the heating box along with the oxidant, heating the water body in the heating box, selectively adjusting the telescopic degree of the electric telescopic rod according to the temperature requirement, and further adjusting the pressure between the heat insulation sliding plate and the water body in the heating box, so that the purpose of adjusting the steam temperature in the heating box is achieved, when the interior of the inner tank needs to be subjected to condensation treatment, two groups of electronic control valves and the heating interlayer are simultaneously closed, and at the moment, the hot steam in the heating box is limited in a space formed by the heating box and the heat insulation sliding plate, so that the refrigeration efficiency of the air supply hose cannot be influenced;
s3, wherein the oxidant is sodium hypobromite or hypobromous acid, and the mass ratio of the solvent in S1 to the ethyl 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-carboxylate is 3-10: 1, the mass ratio of dimethylformamide or dimethylacetamide to R-ClnBrm in the solvent is 1: 1- -3: 1, bromine and ethyl 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-carboxylate in a molar ratio of 1.5 to 3.5: 1, the molar ratio of bromine to the auxiliary brominating agent is 1-10: 1;
s4, heating the inner tank by the obtained steam meeting the temperature requirement through a heat conducting hose, further realizing the oxidation reaction of the reaction mixed liquid in the inner tank, separating the oxidation product, and hydrolyzing and acidifying to obtain 3-bromo-1- (3-chloropyridine-2-yl) -1H-pyrazole-5-formic acid;
s5 in S2, the molar ratio of oxidizing agent to the initially charged ethyl 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-carboxylate is 0.1 — 1.2: 1, the reaction temperature is 70-120 ℃, the oxidation reaction pressure is 0-1.2 MPa, when the reaction pressure in the inner tank needs to be adjusted, the inner tank can be pressurized by a pressure pump, the electromagnetic valve is closed in the secondary process, the reaction pressure in the inner tank can be detected by a pressure sensor, the output power of the pressure pump is further adjusted, when the pressure reduction treatment is needed for the subsequent reaction operation in the inner tank, the electromagnetic valve can be opened, the pressure relief treatment is carried out in the inner tank, and then redundant tail gas enters the tail gas collecting box;
s6, after the tail gas in the inner tank enters the first collecting cavity, the tail gas sequentially enters the second collecting cavity, the third collecting cavity and the fourth collecting cavity through the through pipes in a one-way mode, and the dissolving, extracting, collecting and processing of different gases in the tail gas mixed gas are achieved according to the difference of storage solutions in the first collecting cavity, the second collecting cavity, the third collecting cavity and the fourth collecting cavity.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the heating interlayer in the heating box is started through the heating box, the heating interlayer, the heat insulation sliding plate, the electric telescopic rod, the heat conduction hose, the electronic control valve and the second one-way valve, the water body in the heating box is subjected to temperature rise treatment, and the expansion degree of the electric telescopic rod is selectively adjusted, so that the purpose of adjusting the steam temperature in the heating box is realized, and when the interior of the inner tank is required to be subjected to condensation treatment, two groups of electronic control valves and the heating interlayer are simultaneously closed, so that the refrigeration efficiency of the air supply hose is not influenced.
2. According to the invention, the tail gas collecting box, the first collecting cavity, the second collecting cavity, the third collecting cavity, the fourth collecting cavity, the cross partition frame, the through pipe, the first one-way valve and the breathable film are arranged, after the tail gas in the inner tank enters the first collecting cavity, the tail gas sequentially enters the second collecting cavity, the third collecting cavity and the fourth collecting cavity through the through pipe in a one-way mode, and the dissolving, extracting and collecting treatment of different gases in the tail gas mixed gas is realized according to different storage solutions in the first collecting cavity, the second collecting cavity, the third collecting cavity and the fourth collecting cavity.
3. According to the invention, the pressurization pump, the gas guide pipe, the gas outlet pipe, the pressure sensor, the third one-way valve and the electromagnetic valve are arranged, the gas after pressurization treatment can be sent into the inner tank through the gas guide pipe by the pressurization pump so as to meet the pressure requirement required by the related chemical reaction inside the inner tank, the electromagnetic valve is opened when the pressure inside the inner tank is required to be reduced, and the redundant gas inside the inner tank is transferred to the inside of the tail gas collecting box along the gas outlet pipe in a one-way manner, so that the pressure reduction treatment is realized.
4. The condenser, the air supply hose, the first heat insulation plate, the second heat insulation plate, the magnetic stripe and the electromagnet are arranged, and the sliding storage of the first heat insulation plate and the second heat insulation plate can be realized by adjusting the direction of the current connected to the electromagnet, so that the intermittent heat insulation protection is formed for the air supply hose, and the interference of the heat conduction hose is avoided.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a schematic view of the internal installation structure of the driving motor, the stirring rod and the preparation reaction kettle of the invention;
FIG. 3 is a schematic view of the internal installation structure of the exhaust gas collection box according to the present invention;
FIG. 4 is a schematic view of the internal structure of the pipe of the present invention;
FIG. 5 is a schematic view of the installation structure of the air hose of the present invention and the first and second heat insulation plates;
fig. 6 is a schematic view illustrating a structure of an air supply hose according to the present invention;
FIG. 7 is a schematic view of a heating cabinet mounting structure of the present invention;
FIG. 8 is a schematic view of the installation structure of the airway tube and the exit tube of the present invention.
In the figure: 1. preparing a reaction kettle; 101. an inner tank; 102. heat treating the interlayer; 2. a drive motor; 201. a stirring paddle; 3. a tail gas collection box; 301. a first collection cavity; 302. a second collection cavity; 303. a third collection cavity; 304. a fourth collection cavity; 305. a cross-shaped partition plate frame; 306. pipe passing; 307. a first check valve; 308. a gas permeable membrane; 4. a condenser; 401. an air supply hose; 402. a first heat insulation plate; 403. a second heat insulation plate; 404. a magnetic strip; 405. an electromagnet; 406. an electronic thermometer; 5. a heating box; 501. heating the interlayer; 502. a heat insulation slide plate; 503. an electric telescopic rod; 504. a heat conducting hose; 505. an electronic control valve; 506. a second one-way valve; 6. sealing the top cover; 601. a first feed port; 602. a second feed port; 603. a third feed inlet; 604. a fourth feed port; 7. a pressure pump; 701. an air duct; 702. an air outlet pipe; 703. a pressure sensor; 704. a third check valve; 705. an electromagnetic valve; 8. a discharge pipe; 9. an exhaust pipe; 10. an electronic display screen.
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. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front", "rear", "both ends", "one end", "the other end", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "connected," and the like are to be construed broadly, such as "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example one
Referring to fig. 1 and 7, an embodiment of the present invention: an apparatus for efficiently producing pyrazole carboxylic acid comprises a preparation reaction kettle 1 and a heating box 5, wherein a tail gas collecting box 3 and the heating box 5 are arranged on the surface of the preparation reaction kettle 1, the heating box 5 is positioned above the tail gas collecting box 3, a condenser 4 and a pressure pump 7 are arranged on the surface of the preparation reaction kettle 1, the pressure pump 7 is positioned below the condenser 4, and the tail gas collecting box 3 is positioned on one side of the pressure pump 7;
The inner tank 101 is arranged in the preparation reaction kettle 1, the tail end of the gas guide pipe 701 extends into the inner tank 101, a heat treatment interlayer 102 is arranged in a space formed by the inner tank 101 and the inner wall of the preparation reaction kettle 1, the heat conduction hose 504 and the gas supply hose 401 are both located in the heat treatment interlayer 102, a temperature sensor is arranged on the inner wall of the inner tank 101, and the temperature sensor is electrically connected with the electronic display screen 10.
Specifically, the top of the electric telescopic rod 503 is connected with the top of the heating box 5, and the heat conducting hose 504 can form a surrounding type surrounding treatment for the inner tank 101;
starting the heating interlayer 501, so that a water body in the heating box 5 is heated and evaporated, then closing the two groups of electronic control valves 505, adjusting the electric telescopic rod 503, so that the heat insulation sliding plate 502 slides up and down along the inner wall of the heating box 5, so as to adjust the bottom of the heat insulation sliding plate 502 and the water surface in the heating box 5 to form a fixed space, and as the heating operation in the heating interlayer 501 continues, under the condition of constant space, the heat of steam gradually rises along with the increase of heat, and after the corresponding temperature requirement is met, the two groups of electronic control valves 505 can be opened, so that the steam in the heating box 5 is transferred to the heat conducting hose 504, and further, the corresponding temperature rise treatment is carried out on the interior of the inner tank 101;
in the process, the second check valve 506 assists steam to realize one-way conveying, and further when the condenser 4 needs to be started to perform refrigeration operation on the inside of the inner tank 101 in the follow-up process, the heating interlayer 501 and the two sets of electronic control valves 505 can be closed first, and after the steam inside the heating box 5 is cooled and condensed into water drops, the two sets of electronic control valves 505 are opened, so that the high-pressure hot steam remaining inside the heat-conducting hose 504 is extruded and conveyed to the inside of the heating box 5, and the influence of the residual heat inside the heat-conducting hose 504 on the condensing efficiency of the condenser 4 is avoided.
In the heating process, the temperature inside the inner tank 101 can be visually displayed through the electronic display screen 10, so that an operator can conveniently master the working power of the heating interlayer 501 in real time during heating operation.
Example two
Referring to fig. 1, fig. 3 and fig. 4, an embodiment of the present invention: the utility model provides an equipment of high-efficient production pyrazole formic acid, including tail gas collection box 3, the internally mounted of tail gas collection box 3 has cross partition frame 305, the internal space of tail gas collection box 3 is divided into four independent spaces through cross partition frame 305 and first collects cavity 301, the second collects cavity 302, third and collect cavity 303 and fourth and collect cavity 304, and first collection cavity 301, the second collects cavity 302, third and collect cavity 303 and fourth and collect cavity 304 anticlockwise arrangement, the inside of cross partition frame 305 runs through and installs siphunculus 306, second collects cavity 302 and third and collect cavity 303, first collection cavity 301 and second and collect cavity 302, third and collect cavity 303 and fourth and collect cavity 304 and all connect through siphunculus 306, the internally mounted of siphunculus 306 has ventilated membrane 308 and the first check valve 307 of parallel arrangement.
The surface mounting of box 3 is collected to tail gas has row material pipe 8 that the matrix was arranged, and the tail end of four groups of row material pipes 8 extends into first collection cavity 301, second collection cavity 302, the inside of collecting cavity 303 and fourth collection cavity 304 respectively, and the valve is all installed on the surface of every group row material pipe 8, and blast pipe 9 is installed at the top of box 3 is collected to tail gas, and the tail end of blast pipe 9 runs through the inside that extends to first collection cavity 301.
Specifically, an organic solvent is stored in the fourth collecting cavity 304, clear water is stored in the third collecting cavity 303, an acidic solution is stored in the second collecting cavity 302, and an alkaline solution is stored in the first collecting cavity 301;
the gas-permeable membrane 308 only allows gas to pass through, so that after the tail gas in the gas outlet pipe 702 enters the fourth collecting cavity 304, the gas dissolved in the organic solvent in the mixed tail gas can be absorbed under the cooperation of the first check valve 307 and the gas-permeable membrane 308 in the through pipe 306, and then the gas is transferred to the third collecting cavity 303 through the through pipe 306, and after the gas dissolved in water is absorbed, the gas is transferred to the second collecting cavity 302 through the through pipe 306 to absorb the alkaline gas in the mixed gas, and finally the alkaline solution in the first collecting cavity 301 absorbs the residual acidic gas in the mixed gas;
after the quadruple dissolution absorption reaction treatment, residual gas in the tail gas is discharged through the exhaust pipe 9, and the corresponding valve on the surface of the discharge pipe 8 is opened, so that the liquid in the first collection cavity 301, the second collection cavity 302, the third collection cavity 303 and the fourth collection cavity 304 can be taken out, and the collection purpose is realized.
EXAMPLE III
Referring to fig. 1, fig. 2 and fig. 8, an embodiment of the present invention: the utility model provides an equipment of high-efficient production pyrazole formic acid, including preparation reation kettle 1, the output of force (forcing) pump 7 is connected with air duct 701, the surface mounting of air duct 701 has outlet duct 702, and the tail end of outlet duct 702 extends into the inside of fourth collection cavity 304, the surface mounting of outlet duct 702 has solenoid valve 705, third check valve 704 is all installed to the inside of outlet duct 702 and air duct 701, the third check valve 704 of the inside of air duct 701 is located the place ahead of the junction of air duct 701 and outlet duct 702, the tail end surface mounting of air duct 701 has pressure sensors 703.
Specifically, the pressurized gas can be sent into the inner tank 101 through the gas guide pipe 701 by the pressure pump 7 to meet the pressure requirement required for the relevant chemical reaction inside the inner tank 101, and the real-time pressure inside the inner tank 101 is detected by the pressure sensor 703 at the tail end, so that the operator can adjust the pressurizing power of the pressure pump 7 in time;
after the pressurization, open solenoid valve 705 when needing to carry out the decompression processing to inner tank 101 inside, because the inside third check valve 704 of air duct 701 is located the place ahead of air duct 701 and outlet duct 702 junction, when inner tank 101 is inside to carry out the decompression operation, inside unnecessary gas is gone back to the inside third check valve 704 of air duct 701 through the air duct 701 front end and is gone out the back, inside along the one-way transfer of outlet duct 702 to tail gas collection box 3, realizes the decompression processing.
Example four
Referring to fig. 1, fig. 2, fig. 5 and fig. 6, an embodiment of the present invention: the utility model provides an equipment of high-efficient production pyrazole formic acid, including condenser 4, the surface mounting of condenser 4 has the hose 401 of sending gas of equidistance arrangement, the surface of sending gas hose 401 encircles and installs No. two insulation boards 403, the inner wall of No. two insulation boards 403 installs electro-magnet 405, No. two insulation boards 403's inside slidable mounting has insulation board 402, the width of insulation board 402 is less than No. two insulation boards 403, the tail end of insulation board 402 is connected with magnetic stripe 404, the width of magnetic stripe 404 is the same with the width of No. two insulation boards 403, No. two insulation boards 403's surface mounting has electronic thermometer 406, and electronic thermometer 406 and electronic display screen 10 electric connection.
Specifically, the air supply hose 401 is wound around the surface of the inner tank 101 and arranged at an interval with the heat conduction hose 504, after the condenser 4 is started, the internal cold air enters the heat treatment interlayer 102 through the air supply hose 401, the electromagnet 405 is started at the moment, an electromagnetic adsorption effect can be generated, the magnetic strip 404 is close to the electromagnet 405, the first heat insulation plate 402 is further slid into the second heat insulation plate 403, the surface of the air supply hose 401 loses the heat insulation protection when the first heat insulation plate 402 and the second heat insulation plate 403 form enclosure, and the heat exchange between the cold air in the air supply hose 401 and the inside of the heat treatment interlayer 102 is facilitated, so that the corresponding cooling is realized;
when the inner tank 101 needs to be heated, the direction of current access of the electromagnet 405 is changed, that is, the direction of electromagnetic adsorption can be changed, so that the magnetic strip 404 is far away from the electromagnet 405, the first heat insulation plate 402 and the second heat insulation plate 403 are completely stretched, the surface of the air supply hose 401 is subjected to enclosed heat insulation treatment, and the heat transfer of the heat conduction hose 504 is avoided;
during the cooling process, the temperature inside the thermal treatment jacket 102 can be detected by the electronic thermometer 406, thereby indirectly knowing the temperature inside the inner tank 101.
The top of the preparation reaction kettle 1 is provided with a seal top cover 6, the top of the seal top cover 6 is provided with a first feed inlet 601, a second feed inlet 602, a third feed inlet 603 and a fourth feed inlet 604 in a matrix manner, the first feed inlet 601 and the second feed inlet 602 are symmetrically arranged, the third feed inlet 603 and the fourth feed inlet 604 are symmetrically arranged, the tail ends of the first feed inlet 601, the second feed inlet 602, the third feed inlet 603 and the fourth feed inlet 604 extend into the inner tank 101, the top of the seal top cover 6 is provided with a driving motor 2, the output end of the driving motor 2 is provided with a stirring paddle 201, and the stirring paddle 201 is positioned in the inner tank 101.
Specifically, the arrangement of the first feed inlet 601, the second feed inlet 602, the third feed inlet 603 and the fourth feed inlet 604 can enable operators to separately feed multiple reactants when preparing the pyrazolecarboxylic acid, so that mixed feeding is avoided;
in addition, in the reaction process, the driving motor 2 is started to drive the stirring paddle 201 to rotate, so that the dissolution and the mixing of the mixture in the inner tank 101 can be accelerated.
EXAMPLE five
800g of dimethylformamide and 350g of chlorobromomethane are added to the inner tank 101, ethyl 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-carboxylate (136.8 g, 97.51%, 0.495 mol) is added, the temperature is reduced to 20 ℃ with stirring, and bromine (125.6 g, 99.0%, 0.778 mol) is carefully added. After the temperature is kept at 20-30 ℃ for 90 minutes, sodium hypobromite (20%, 87.2g, 0.18 mol) is added, the inner tank 101 is sealed, the temperature is raised to about 120 ℃ after stirring for 60 minutes, and the pressure is raised to 0.18 MPa. Keeping the temperature for 150 minutes, and detecting that the content of 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-ethyl formate is 0.07 percent and the content of 3-bromo-1- (3-chloropyridin-2-yl) -4, 5-dihydro-1H-pyrazoline-5-ethyl formate is 0.11 percent. Ending heat preservation, releasing the pressure to normal pressure through a condenser, evaporating to remove the chlorobromomethane which is insoluble in water and water, then carrying out pressure filtration at 70-80 ℃, washing a filter cake by 30g of dimethylformamide, combining a filtrate and a washing solution, controlling the temperature to be less than 85 ℃, evaporating out the dimethylformamide under reduced pressure, adding 200g of water into a kettle substrate material, then cooling to 5 ℃, carrying out heat preservation for 1 hour, carrying out pressure filtration, rinsing the filter cake to be white for multiple times by 100g of cold methanol at the temperature of below 10 ℃, drying to obtain 154.3g of white solid powder, detecting the content of 3-bromo-1- (3-chloropyridine-2-yl) -1H-pyrazole-5-ethyl formate by 98.20 percent and calculating by using ethyl 2- (3-chloropyridine-2-yl) -5-oxo-1H-pyrazolidine-3-ethyl formate, the total mole yield of bromination and oxidation is 92.68%.
EXAMPLE six
Acetonitrile 180.1g, ethyl 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-carboxylate (56.5 g, 97.65%, 0.205 mol), phosphorus oxybromide (38.1 g, 99.15%, 0.132 mol) were added to a four-necked flask. Stirring at normal temperature for 30min, heating to reflux, reflux reacting for 120min, and detecting ethyl 2- (3-chloropyridine-2-yl) -5-oxo-1H-pyrazolidine-3-carboxylate content to 0.25%. Transferring the materials into a rotary evaporator, controlling the temperature not to exceed 80 ℃, and distilling out the acetonitrile. After acetonitrile is evaporated to dryness, 120g of water is added into a bottle, stirring is carried out, 36.8g of sodium bicarbonate is added to neutralize the solution until the pH value is 6.9, stirring is carried out for 30min at the temperature of 30-40 ℃, suction filtration and filter cake drying are carried out, and white-like powder, namely 3-bromo-1- (3-chloropyridin-2-yl) -4, 5-dihydro-1H-pyrazoline-5-ethyl formate (66.5 g, 99.47 percent, 0.199 mol) and the bromination yield is 97.16 percent is obtained.
EXAMPLE seven
192g of acetonitrile, 66.5g of ethyl 3-bromo-1- (3-chloropyridin-2-yl) -4, 5-dihydro-1H-pyrazoline-5-carboxylate (66.47 mol, 99.47 mol) obtained in the sixth example, was added to a flask, potassium persulfate (72.5 g, 98.18 mol, 0.263 mol) and 98% sulfuric acid (48.7 g, 0.487 mol) were added in portions at 60 ℃ and the temperature was raised after the addition, the flask was cooled in a water bath at 70 ℃ to 80 ℃ and then kept warm for 65min after the addition, 0.22% of ethyl 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-carboxylate was detected, and after removing 130g of acetonitrile under reduced pressure, 400g of water was added to the flask, the flask was further stirred and cooled to 20 ℃ for 30min, suction filtration was carried out, the cake was washed with water to pH 6.8, after drying, 68.3g of a grayish green solid (the content of 3-bromo-1- (3-chloropyridin-2-yl) -1H-pyrazole-5-carboxylic acid ethyl ester is 86.06 percent, 0.178 mol) is obtained, and the yield is 89.46 percent. 68.3g of gray-green solid is added with 100g of ethanol, heated to 70 ℃, stirred and cooled to 0 ℃, kept warm for 30min and filtered to obtain 47.8g of white powdery crystals (the content of 3-bromo-1- (3-chloropyridin-2-yl) -1H-pyrazole-5-ethyl formate is 96.01 percent, and 0.139 mol).
Synthesis of ethyl 3-bromo-1- (3-chloropyridin-2-yl) -1H-pyrazole-5-carboxylate from ethyl 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-carboxylate in two steps, six and seven, total molar yield 86.92%, e.g. ethyl 3-bromo-1- (3-chloropyridin-2-yl) -1H-pyrazole-5-carboxylate was refined to 95% or more, total molar yield 67.86%.
Example eight
950g of dimethylacetamide and 380g of 1, 1-dibromoethane are added into an inner tank 101, ethyl 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-carboxylate (150.2 g, 97.45 mol and 0.543 mol) is added, the temperature is reduced to 18 ℃ by stirring, bromine (149.8 g, 99.1 mol and 0.929 mol) is carefully added, the temperature is maintained at 20 ℃ to 30 ℃ for 55 minutes, sodium hypobromite (20%, 149.6g and 0.309 mol) is added, the inner tank 101 is sealed, the temperature is increased to 120 ℃ by stirring for 60 minutes, and the pressure is increased to 0.13 MPa. Keeping the temperature for 120 minutes, detecting the content of 0.02 percent of 2- (3-chloropyridine-2-yl) -5-oxo-1H-pyrazolidine-3-ethyl formate and the content of 0.08 percent of 3-bromo-1- (3-chloropyridine-2-yl) -4, 5-dihydro-1H-pyrazoline-5-ethyl formate, ending the heat preservation, releasing the pressure to the normal pressure through a condenser, evaporating dibromoethane and water, then carrying out pressure filtration at 70-80 ℃, washing a filter cake with 50g of dimethylacetamide, combining filtrate and washing liquid, controlling the temperature to be less than 85 ℃, evaporating the dimethylacetamide under reduced pressure, adding 250g of water into a kettle substrate material, then cooling to 5 ℃, keeping the temperature for 1 hour, carrying out pressure filtration, rinsing the filter cake to be white by 100g of cold methanol below 10 ℃ for multiple times, after drying, 171.2g of white solid powder was obtained, and the content of ethyl 3-bromo-1- (3-chloropyridin-2-yl) -1H-pyrazole-5-carboxylate was determined to be 98.32%, based on ethyl 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-carboxylate, the total molar yield of bromination and oxidation was 93.82%
The working steps of the improved method are as follows:
s1, adding a solvent into the inner tank 101 through the first feed port 601, immediately feeding 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-ethyl formate into the inner tank 101 through the second feed port 602, and then adding a brominating agent through the third feed port 603 to perform bromination reaction, wherein the solvent is a mixture of dimethylformamide or dimethylacetamide and R-ClnBrm, R-is C1-C3 alkyl or phenyl, n and m are 0 or natural numbers of 1-8, the brominating agent is a mixture of bromine and an auxiliary brominating agent, and the auxiliary brominating agent is a mixture of bromine and the auxiliary brominating agent
(N-bromoamide),
One or more of (N-bromosuccinimide), phosphorus oxybromide, phosphorus tribromide and thionyl bromide;
s2, adding an oxidant into the S1 reaction liquid through the fourth feed inlet 604, starting the heating interlayer 501 in the heating box 5 along with the oxidant, heating the water in the heating box 5, selectively adjusting the expansion degree of the electric telescopic rod 503 according to the temperature requirement, and further adjusting the pressure between the heat insulation sliding plate 502 and the water in the heating box 5, so as to achieve the purpose of adjusting the temperature of the steam in the heating box 5, and simultaneously closing the two groups of electronic control valves 505 and the heating interlayer 501 when the interior of the inner tank 101 needs to be subjected to condensation treatment, so that the hot steam in the heating box 5 is limited in the space formed by the heating box 5 and the heat insulation sliding plate 502, and the refrigeration efficiency of the air supply hose 401 cannot be influenced;
s3, wherein the oxidant is sodium hypobromite or hypobromous acid, and the mass ratio of the solvent in S1 to the ethyl 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-carboxylate is 3-10: 1, the mass ratio of dimethylformamide or dimethylacetamide to R-ClnBrm in the solvent is 1: 1- -3: 1, bromine and ethyl 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-carboxylate in a molar ratio of 1.5 to 3.5: 1, the molar ratio of bromine to the auxiliary brominating agent is 1-10: 1;
s4, heating the inner tank 101 by the obtained steam meeting the temperature requirement through the heat conducting hose 504, further realizing the oxidation reaction of the reaction mixed liquid in the inner tank 101, separating the oxidation product, and hydrolyzing and acidifying to obtain 3-bromo-1- (3-chloropyridine-2-yl) -1H-pyrazole-5-formic acid;
s5 in S2, the molar ratio of oxidizing agent to the initially charged ethyl 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-carboxylate is 0.1 — 1.2: 1, the reaction temperature is 70-120 ℃, the oxidation reaction pressure is 0-1.2 MPa, when the reaction pressure in the inner tank 101 needs to be adjusted, the pressure pump 7 can be used for pressurizing the inner tank 101, the electromagnetic valve 705 is closed in the next process, the reaction pressure in the inner tank 101 can be detected through the pressure sensor 703, the output power of the pressure pump 7 is further adjusted, when the pressure reduction treatment is needed for the subsequent reaction operation in the inner tank 101, the electromagnetic valve 705 can be opened, the pressure relief treatment is carried out in the inner tank 101, and then the redundant tail gas enters the tail gas collecting box 3;
s6, after the tail gas in the inner tank 101 enters the first collection cavity 301, the tail gas firstly and secondly enters the second collection cavity 302, the third collection cavity 303 and the fourth collection cavity 304 through the through pipe 306 in a one-way mode, and dissolution, extraction, collection and treatment of different gases in the tail gas mixed gas are achieved according to the difference of storage solutions in the first collection cavity 301, the second collection cavity 302, the third collection cavity 303 and the fourth collection cavity 304.
The working principle is as follows: adding a solvent into the inner tank 101 through a first feed port 601, immediately feeding 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-ethyl formate into the inner tank 101 through a second feed port 602, and then adding a brominating agent through a third feed port 603 to perform bromination reaction, wherein the solvent is a mixture of dimethylformamide or dimethylacetamide and R-ClnBrm, R-is C1-C3 alkyl or phenyl, N and m are 0 or natural numbers of 1 to 8, the brominating agent is a mixture of bromine and an auxiliary brominating agent, and the auxiliary brominating agent is one or more of (N-bromoamide), (N-bromosuccinimide), phosphorus oxybromide, phosphorus tribromide and thionyl bromide;
then, an oxidant is added into the S1 reaction solution through the fourth feed inlet 604, the heating interlayer 501 inside the heating box 5 is started along with the oxidant, the water inside the heating box 5 is heated, the expansion degree of the electric telescopic rod 503 is selectively adjusted according to the temperature requirement, and the pressure between the heat insulation sliding plate 502 and the water inside the heating box 5 is further adjusted, so that the purpose of adjusting the temperature of steam inside the heating box 5 is achieved, when the interior of the inner tank 101 needs to be condensed, the two groups of electronic control valves 505 and the heating interlayer 501 are simultaneously closed, and at the moment, the hot steam inside the heating box 5 is limited in the space formed by the heating box 5 and the heat insulation sliding plate 502, so that the refrigeration efficiency of the air supply hose 401 is not affected;
the obtained steam meeting the temperature requirement can be used for heating the inner tank 101 through the heat conducting hose 504, so that the oxidation reaction of the reaction mixed liquid in the inner tank 101 is realized, and after the oxidation product is separated, the 3-bromine-1- (3-chloropyridine-2-yl) -1H-pyrazole-5-formic acid is obtained through hydrolysis and acidification;
when the reaction pressure in the inner tank 101 needs to be adjusted, the pressure pump 7 can be used for pressurizing the interior of the inner tank 101, the electromagnetic valve 705 is closed in the secondary process, the pressure sensor 703 can be used for detecting the reaction pressure in the interior of the inner tank 101, the output power of the pressure pump 7 is further adjusted, and when the pressure reduction treatment is needed in the subsequent reaction operation in the interior of the inner tank 101, the electromagnetic valve 705 can be opened, so that the pressure relief treatment is performed in the interior of the inner tank 101, and then the redundant tail gas enters the interior of the tail gas collecting box 3;
inside tail gas of inner tank 101 gets into first collection cavity 301 inside back, and it is inside first back to collect cavity 302, third collection cavity 303 and fourth collection cavity 304 through the one-way entering of siphunculus 306, collects the difference of cavity 302 and third collection cavity 303 and the inside deposit solution of fourth collection cavity 304 according to first collection cavity 301, second, realizes dissolving extraction collection processing of different gases in the tail gas mist.
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 (10)
1. The equipment for efficiently producing the pyrazole formic acid comprises a preparation reaction kettle (1), and is characterized in that: the device comprises a preparation reaction kettle (1), a tail gas collecting box (3) and a heating box (5) are mounted on the surface of the preparation reaction kettle (1), the heating box (5) is located above the tail gas collecting box (3), a condenser (4) and a pressure pump (7) are mounted on the surface of the preparation reaction kettle (1), the pressure pump (7) is located below the condenser (4), and the tail gas collecting box (3) is located on one side of the pressure pump (7);
a heating interlayer (501) is arranged in the heating box (5), a heat conduction hose (504) is installed on the inner wall of the heating box (5) in a penetrating mode, a second one-way valve (506) is installed inside the heat conduction hose (504), the tail end of the heat conduction hose (504) extends back to the inside of the heating box (5), two groups of electronic control valves (505) which are arranged at equal intervals are installed on the surface of the heat conduction hose (504), a heat insulation sliding plate (502) is installed on the inner wall of the heating box (5), and electric telescopic rods (503) are installed at four corners of the top of the heat insulation sliding plate (502);
and an electronic display screen (10) is arranged on the surface of the heating box (5).
2. The apparatus for efficiently producing pyrazolecarboxylic acid according to claim 1, wherein: a cross partition rack (305) is arranged in the tail gas collecting box (3), the internal space of the tail gas collecting box (3) is divided into a first collecting cavity (301), a second collecting cavity (302), a third collecting cavity (303) and a fourth collecting cavity (304) through the cross partition rack (305), and the first (301), second (302), third (303) and fourth (304) collecting cavities are arranged counter-clockwise, a through pipe (306) is arranged in the cross partition rack (305) in a penetrating way, the second collection cavity (302) and the third collection cavity (303), the first collection cavity (301) and the second collection cavity (302), the third collection cavity (303) and the fourth collection cavity (304) are all connected through the through pipe (306), the inside of the through pipe (306) is provided with a gas-permeable membrane (308) and a first one-way valve (307) which are arranged in parallel.
3. The apparatus for efficiently producing pyrazolecarboxylic acid according to claim 1, wherein: the output of force (forcing) pump (7) is connected with air duct (701), the surface mounting of air duct (701) has outlet duct (702), and the tail end of outlet duct (702) extends into the inside of fourth collection cavity (304), the surface mounting of outlet duct (702) has solenoid valve (705), third check valve (704) are all installed to the inside of outlet duct (702) and air duct (701), third check valve (704) of air duct (701) inside are located the place ahead of air duct (701) and outlet duct (702) junction, the tail end surface mounting of air duct (701) has pressure sensors (703).
4. The apparatus for efficiently producing pyrazolecarboxylic acid according to claim 1, wherein: the surface mounting of condenser (4) has air hose (401) of sending that the equidistance was arranged, the surface of sending air hose (401) is encircleed and is installed No. two insulation boards (403), electro-magnet (405) are installed to the inner wall of No. two insulation boards (403), the inside slidable mounting of No. two insulation boards (403) has insulation board (402), the width of insulation board (402) is less than No. two insulation boards (403), the trailing end connection of an insulation board (402) has magnetic stripe (404), the width of magnetic stripe (404) is the same with the width of No. two insulation boards (403), the surface mounting of No. two insulation boards (403) has electronic thermometer (406), and electronic thermometer (406) and electronic display screen (10) electric connection.
5. The apparatus for efficiently producing pyrazolecarboxylic acid according to claim 1, wherein: the internally mounted of preparation reation kettle (1) has inner tank (101), and the tail end of air duct (701) extends into the inside of inner tank (101), the space that inner tank (101) and preparation reation kettle (1) inner wall pressed from both sides becomes is heat treatment intermediate layer (102), and heat conduction hose (504) and air feed hose (401) all are located the inside of heat treatment intermediate layer (102), the temperature-sensing ware is installed to the inner wall of inner tank (101), and temperature-sensing ware and electronic display screen (10) electric connection.
6. The apparatus for efficiently producing pyrazolecarboxylic acid according to claim 1, wherein: seal cap (6) are installed at the top of preparation reation kettle (1), first feed inlet (601), second feed inlet (602), third feed inlet (603) and fourth feed inlet (604) have been arranged to the top matrix of seal cap (6), first feed inlet (601) and second feed inlet (602) symmetrical arrangement, third feed inlet (603) and fourth feed inlet (604) symmetrical arrangement, the tail end of first feed inlet (601), second feed inlet (602), third feed inlet (603) and fourth feed inlet (604) all extends into the inside of inner tank (101).
7. The apparatus for efficiently producing pyrazolecarboxylic acid according to claim 6, wherein: driving motor (2) are installed at the top of seal cover (6), stirring rake (201) are installed to the output of driving motor (2), and stirring rake (201) are located the inside of inner tank (101).
8. The apparatus for efficiently producing pyrazolecarboxylic acid according to claim 1, wherein: the surface mounting of box (3) is collected to tail gas has row material pipe (8) that the matrix was arranged, and the tail end of four groups of row material pipes (8) extends into the inside that first collection cavity (301), second were collected cavity (302), third were collected cavity (303) and fourth were collected cavity (304), every group row the surface of arranging material pipe (8) all installs the valve.
9. The apparatus for efficiently producing pyrazolecarboxylic acid according to claim 1, wherein: exhaust pipe (9) are installed at the top of tail gas collection box (3), and the tail end of exhaust pipe (9) runs through the inside that extends to first collection cavity (301).
10. An improved process for the efficient production of pyrazolecarboxylic acids using an apparatus according to any of claims 1 to 9, characterized in that the process comprises the following working steps:
s1, adding solvent into the inner tank (101) through the first feeding hole (601), and then adding 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyridineThe oxazolidine-3-ethyl formate is put into an inner tank (101) through a second feeding hole (602), then a brominating agent is added through a third feeding hole (603) for bromination reaction, wherein the solvent is a mixture of dimethylformamide or dimethylacetamide and R-ClnBrm, R-is C1-C3 alkyl or phenyl, n and m are 0 or natural numbers of 1-8, the brominating agent is a mixture of bromine and an auxiliary brominating agent, and the auxiliary brominating agent is bromine
(N-bromoamide),
One or more of (N-bromosuccinimide), phosphorus oxybromide, phosphorus tribromide and thionyl bromide;
s2, adding an oxidant into the S1 reaction liquid through a fourth feed inlet (604), starting a heating interlayer (501) in the heating box (5) along with the oxidant, heating the water body in the heating box (5), selectively adjusting the expansion degree of an electric telescopic rod (503) according to the temperature requirement, and further adjusting the pressure between the heat insulation sliding plate (502) and the water body in the heating box (5), so that the purpose of adjusting the steam temperature in the heating box (5) is achieved, and when the interior of the inner tank (101) needs to be subjected to condensation treatment, two groups of electronic control valves (505) and the heating interlayer (501) are simultaneously closed, at the moment, the hot steam in the heating box (5) is limited in a space formed by the heating box (5) and the heat insulation sliding plate (502), and the refrigeration efficiency of the air supply hose (401) cannot be influenced;
s3, wherein the oxidant is sodium hypobromite or hypobromous acid, and the mass ratio of the solvent in S1 to the ethyl 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-carboxylate is 3-10: 1, the mass ratio of dimethylformamide or dimethylacetamide to R-ClnBrm in the solvent is 1: 1- -3: 1, bromine and ethyl 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-carboxylate in a molar ratio of 1.5 to 3.5: 1, the molar ratio of bromine to the auxiliary brominating agent is 1-10: 1;
s4, heating the inner tank (101) by the obtained steam meeting the temperature requirement through a heat conducting hose (504), further realizing the oxidation reaction of the reaction mixed liquid in the inner tank (101), separating the oxidation product, and hydrolyzing and acidifying to obtain 3-bromo-1- (3-chloropyridine-2-yl) -1H-pyrazole-5-formic acid;
s5 in S2, the molar ratio of oxidizing agent to the initially charged ethyl 2- (3-chloropyridin-2-yl) -5-oxo-1H-pyrazolidine-3-carboxylate is 0.1 — 1.2: 1, the reaction temperature is 70-120 ℃, the oxidation reaction pressure is 0-1.2 MPa, when the reaction pressure in the inner tank (101) needs to be adjusted, the inner tank (101) can be pressurized through a pressure pump (7), an electromagnetic valve (705) is closed in the secondary process, the reaction pressure in the inner tank (101) can be detected through a pressure sensor (703), the output power of the pressure pump (7) is further adjusted, when the pressure reduction treatment is needed in the subsequent reaction operation in the inner tank (101), the electromagnetic valve (705) can be opened, the pressure relief treatment is carried out in the inner tank (101), and then the redundant tail gas enters the tail gas collecting box (3);
s6, after tail gas in the inner tank (101) enters the first collection cavity (301), the tail gas enters the second collection cavity (302), the third collection cavity (303) and the fourth collection cavity (304) through the through pipe (306) in a one-way mode, and dissolution, extraction, collection and treatment of different gases in the tail gas mixed gas are achieved according to the difference of storage solutions in the first collection cavity (301), the second collection cavity (302), the third collection cavity (303) and the fourth collection cavity (304).
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| CN214344505U (en) * | 2020-12-04 | 2021-10-08 | 江西天银科技有限公司 | Stills is used in cresol preparation |
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