CN211078991U - Device for synthesizing 4-cyanopyridine - Google Patents
Device for synthesizing 4-cyanopyridine Download PDFInfo
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- CN211078991U CN211078991U CN201921932600.6U CN201921932600U CN211078991U CN 211078991 U CN211078991 U CN 211078991U CN 201921932600 U CN201921932600 U CN 201921932600U CN 211078991 U CN211078991 U CN 211078991U
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Abstract
The utility model provides a device of synthetic 4-cyanopyridine, including vaporizer one, vaporizer two, blender, air pump, fixed bed reactor, spray column, centrifuge one, crystallization kettle and centrifuge two, vaporizer one and vaporizer two are connected with the blender respectively, and the blender is connected with fixed bed reactor, and fixed bed reactor is connected with the spray column, and the spray column bottom is connected with centrifuge one, and centrifuge one is connected with crystallization kettle, and crystallization kettle is connected with centrifuge two. The utility model discloses a proportion of 4-methylpyridine, ammonia and air is adjusted to the blender to the control reaction goes on, improves 4-methylpyridine conversion rate, carries out the solution crystallization through the crystallization kettle, and through centrifugal separation, has further improved the purity of 4-cyanopyridine.
Description
Technical Field
The utility model relates to a chemical industry equipment technical field, in particular to device of synthetic 4-cyanopyridine.
Background
4-cyanopyridine of formula C6H4N2Molecular weight 104.11, a white to pale yellow needle crystal with characteristic odor. Dissolved in ethanol, diethyl ether and benzene. The main application is the intermediate product of medicine and pesticide.
The 4-cyanopyridine is mainly prepared by ammoxidation synthesis of alkylpyridine, gas 4-methylpyridine and ammonia gas are mixed with a certain proportion of air and react under the catalysis condition of a catalyst to generate the 4-cyanopyridine, and the reaction equation is as follows:
the existing reaction equipment and process control conditions are greatly different, the conversion rate of 4-methylpyridine is low, the content of impurities of the synthesized 4-cyanopyridine is high, and the production requirement is difficult to meet. Therefore, a device for synthesizing 4-cyanopyridine is needed to solve the defects of the existing 4-cyanopyridine production.
SUMMERY OF THE UTILITY MODEL
Aiming at the defects of the prior art, the utility model provides a device for synthesizing 4-cyanopyridine, which has high conversion rate of 4-methylpyridine and lower impurity content and improves the production efficiency of 4-cyanopyridine.
The utility model provides a device for synthesizing 4-cyanopyridine, which comprises a first vaporizer, a second vaporizer, a mixer and an air pump, the fixed bed reactor, the spray column, centrifuge I, crystallization kettle and centrifuge II, the gas outlet of the upside of vaporizer I is connected with the gas inlet of the upside of blender one, the gas outlet of the two upsides of vaporizer is connected with the gas inlet of blender upside two, the upside gas inlet of blender is connected with the gas outlet of air pump, the gas outlet of the bottom of blender is connected with fixed bed reactor's top feed inlet, fixed bed reactor's bottom discharge gate is connected with the gas inlet of the left side below of spray column, the liquid outlet of spray column bottom passes through the pipeline and is connected with the left feed inlet of centrifuge I, the discharge gate of a centrifuge bottom is connected with the feed inlet of the top of crystallization kettle, the discharge gate of crystallization kettle below is connected with the feed inlet of.
Preferably, a snakelike vaporization pipe is arranged in the first vaporizer, a heat medium pipe is coated outside the vaporization pipe, a heat medium inlet is formed in the right side of the first vaporizer, a heat medium outlet is formed in the left side of the first vaporizer, the second vaporizer and the first vaporizer are identical in structure, a liquid inlet of the first vaporizer is externally connected with a picoline liquid storage tank, and a liquid inlet of the second vaporizer is externally connected with a liquid ammonia liquid storage tank.
Preferably, the top of the mixer is provided with a first air inlet, a second air inlet and a third air inlet, and the first air inlet, the second air inlet and the third air inlet are respectively provided with an electromagnetic valve.
Preferably, the fixed bed reactor top is equipped with the top and is equipped with the distributor, and the distributor is connected with the feed inlet at fixed bed reactor top, with the inside catalyst fixed bed that is equipped with of fixed bed reactor, both ends are equipped with heat medium import and heat medium export respectively about fixed bed reactor right side outer wall is equipped with, and the fixed bed reactor bottom is equipped with the discharge gate.
Preferably, the spray tower top is equipped with spray set, and the spray tower top is equipped with the cooling water import, and spray set and cooling water access connection are equipped with the air inlet below the left side of spray tower, and the right side top of spray tower is equipped with the gas outlet, and the bottom of spray tower is equipped with the liquid outlet, the external tail gas processing apparatus in gas outlet of spray tower.
Preferably, the inside puddler that is equipped with of crystallization kettle, the puddler is connected with the middle motor in crystallization kettle top, and crystallization kettle top left side is equipped with the feed inlet, and crystallization kettle top right side is equipped with the solvent import, and the crystallization kettle outer wall is equipped with cold and hot medium jacket layer, is equipped with the discharge gate in the middle of the crystallization kettle bottom.
Compared with the prior art, the utility model has the advantages that:
(1) the utility model adopts the vaporizer to vaporize 4-methylpyridine and liquid ammonia and then mix with air through the mixer, the air inlet I, the air inlet II and the air inlet III of the mixer are all provided with control valves, and the proportion of 4-methylpyridine, ammonia and air can be adjusted through the control valves, thereby controlling the reaction and improving the conversion rate of 4-methylpyridine;
(2) the top end of the fixed bed reactor is provided with the distributor, so that the mixed gas can be uniformly distributed to each fixed tube of the catalyst fixed bed, and the reactor is heated by the heat medium more stably and uniformly than the traditional electric heating;
(3) the utility model adopts the characteristic that 4-cyanopyridine has high melting point and is difficult to dissolve in water, the mixed gas after reaction is introduced into a spraying device, the 4-cyanopyridine in the gas can be rapidly cooled and separated out, and the mixed gas enters a centrifugal machine along with slurry for centrifugal separation to obtain a crude product of the 4-cyanopyridine;
(4) the utility model discloses centrifuge one's discharge gate is connected with the feed inlet of crystallization kettle's top, and the inside puddler crystallization kettle top right side that is equipped with of crystallization kettle is equipped with the solvent import, and the crystallization kettle outer wall is equipped with the heat and cold medium jacket layer, dissolves 4-cyanopyridine crude through the solvent, and the rate of cooling is controlled again and 4-cyanopyridine is appeared, and the discharge gate of crystallization kettle below is connected with the feed inlet of centrifuge two's top, obtains 4-cyanopyridine through centrifuge two centrifugation, has improved the purity of 4-cyanopyridine.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic structural diagram of the fixed bed reactor of the present invention;
fig. 3 is a schematic structural diagram of the crystallization kettle of the present invention.
In the figure:
1-a first vaporizer, 2-a second vaporizer, 3-a mixer, 4-an air pump, 5-a fixed bed reactor, 6-a spray tower, 7-a first centrifuge, 8-a crystallization kettle and 9-a second centrifuge.
Detailed Description
In order to better enable those skilled in the art to understand the present invention, the technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiment of the present invention, and it is obvious that the described embodiment is only a part of the embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by a person of ordinary skill in the art without creative efforts belong to the protection scope of the present invention.
As shown in figures 1-3, a device for synthesizing 4-cyanopyridine comprises a first vaporizer 1, a second vaporizer 2, a mixer 3, an air pump 4, a fixed bed reactor 5, a spray tower 6, a first centrifuge 7, a crystallization kettle 8 and a second centrifuge 9, wherein an air outlet at the upper side of the first vaporizer 1 is connected with an air inlet at the upper side of the mixer 3, an air outlet at the upper side of the second vaporizer 2 is connected with an air inlet at the upper side of the mixer 3, an air inlet at the upper side of the mixer 3 is connected with an air outlet of the air pump 4, an air outlet at the bottom of the mixer 3 is connected with a top feed inlet of the fixed bed reactor 5, a bottom discharge port of the fixed bed reactor 5 is connected with an air inlet at the lower left side of the spray tower 6, a liquid outlet at the bottom of the spray tower 6 is connected with the left side of a feed inlet of the centrifuge 7 through, a discharge hole below the crystallization kettle 8 is connected with a feed inlet above the second centrifuge 9.
A snakelike vaporization pipe is arranged in the first vaporizer 1, a heat medium pipe is coated outside the vaporization pipe, a heat medium inlet is formed in the right side of the first vaporizer 1, a heat medium outlet is formed in the left side of the first vaporizer 1, the second vaporizer 2 is identical to the first vaporizer 1 in structure, a liquid inlet of the first vaporizer 1 is externally connected with a 4-methylpyridine liquid storage tank, and a liquid inlet of the second vaporizer 2 is externally connected with a liquid ammonia liquid storage tank.
The top of the mixer 3 is provided with a first air inlet, a second air inlet and a third air inlet, and electromagnetic valves are arranged at the first air inlet, the second air inlet and the third air inlet.
5 tops of fixed bed reactor are equipped with the top and are equipped with the distributor, and the distributor is connected with the feed inlet at 5 tops of fixed bed reactor, with the inside catalyst fixed bed that is equipped with of fixed bed reactor 5, both ends are equipped with heat medium import and heat medium export respectively about 5 right side outer walls of fixed bed reactor are equipped with, and 5 bottoms of fixed bed reactor are equipped with the discharge gate.
6 tops of spray tower are equipped with spray set, and 6 tops of spray tower are equipped with the cooling water import, and spray set and cooling water access connection, the left side below of spray tower 6 is equipped with the air inlet, and the right side top of spray tower 6 is equipped with the gas outlet, and the bottom of spray tower 6 is equipped with the liquid outlet, the external tail gas processing apparatus in gas outlet of spray tower 6.
The inside puddler that is equipped with of crystallization kettle 8, the puddler is connected with the motor in the middle of 8 tops of crystallization kettle, and 8 tops of crystallization kettle left sides are equipped with the feed inlet, and 8 tops of crystallization kettle right sides are equipped with the solvent import, and 8 outer walls of crystallization kettle are equipped with the cooling and heating media jacket layer, are equipped with the discharge gate in the middle of 8 bottoms of crystallization kettle.
The working principle is as follows:
the top of the mixer 3 is provided with a first air inlet, a second air inlet and a third air inlet, electromagnetic valves are arranged at the first air inlet, the second air inlet and the third air inlet, an air outlet at the upper side of the first vaporizer 1 is connected with the first air inlet at the upper side of the mixer 3, an air outlet at the upper side of the second vaporizer 2 is connected with the second air inlet at the upper side of the mixer 3, an air inlet at the upper side of the mixer 3 is connected with an air delivery port of an air pump 4, a liquid inlet of the first vaporizer 1 is externally connected with a 4-methylpyridine liquid storage tank, a liquid ammonia liquid storage tank is externally connected with a liquid ammonia liquid storage tank, the first vaporizer and the second vaporizer are used for vaporizing the 4-methylpyridine and the liquid ammonia and then mixing the vaporized liquid ammonia with air through the.
5 tops of fixed bed reactor are equipped with the top and are equipped with the distributor, the distributor is connected with the feed inlet at 5 tops of fixed bed reactor, with the inside catalyst fixed bed that is equipped with of fixed bed reactor 5, 5 right side outer walls of fixed bed reactor are equipped with about both ends and are equipped with heat medium import and heat medium export respectively, 5 bottoms of fixed bed reactor are equipped with the discharge gate, the distributor can be with each fixed pipe of distribution to the catalyst fixed bed that mist is even, the heat medium import lets in the fused salt and heats the reactor, it is more even stable to heat.
The top end of the spray tower 6 is provided with a spray device, the top of the spray tower 6 is provided with a cooling water inlet, the spray device is connected with the cooling water inlet, the lower part of the left side of the spray tower 6 is provided with an air inlet, the upper part of the right side of the spray tower 6 is provided with an air outlet, the bottom of the spray tower 6 is provided with a liquid outlet, the air outlet of the spray tower 6 is externally connected with a tail gas treatment device, the reacted mixed gas enters the spray tower 6 from the lower part of the left side of the spray tower 6 through the air inlet, the 4-cyanopyridine has a high melting, the mixed gas contacts with cooling gas, 4-cyanopyridine is separated out, and forms slurry with cooling water to be discharged from a liquid outlet at the bottom of the spray tower 6, tail gas is treated by a tail gas treatment device from a gas outlet at the upper right side of the spray tower 6 and then discharged, and the slurry discharged from the liquid outlet at the bottom of the spray tower 6 enters a centrifuge, namely a centrifugal crude product of the 4-cyanopyridine.
The discharge port of the first centrifugal machine 7 is connected with the feed port above the crystallization kettle 8, the stirring rod is arranged inside the crystallization kettle 8, the right side of the top of the crystallization kettle 8 is provided with a solvent inlet, the outer wall of the crystallization kettle 8 is provided with a cooling and heating medium jacket layer, a 4-cyanopyridine crude product is dissolved through a solvent, the cooling speed is controlled to separate out the 4-cyanopyridine, the discharge port below the crystallization kettle 8 is connected with the feed port above the second centrifugal machine 9, and a 4-cyanopyridine finished product is obtained through centrifugation of the second centrifugal machine 9.
When the device is used for synthesizing 4-cyanopyridine, firstly, heating medium is introduced into the first vaporizer 1 and the second vaporizer 2, liquid inlet valves of the first vaporizer 1 and the second vaporizer 2 are opened, 4-methylpyridine and liquid ammonia are introduced, the 4-methylpyridine and the liquid ammonia are vaporized and then introduced into the mixer 3 to be mixed with air, the fully mixed gas is introduced into the fixed bed reactor 5, the heating medium is introduced into the fixed bed reactor to heat the reactor, the mixed gas generates oxidation reaction of the 4-methylpyridine and ammonia gas under the action of a catalyst on the fixed bed when passing through the catalyst fixed bed in the fixed bed reactor 5 to generate the 4-cyanopyridine, the mixed gas containing the 4-cyanopyridine is discharged from a discharge port of the fixed bed reactor 5 and enters the spray tower 6 from an air inlet of the spray tower 6, and cooling water falls down from the spray device, cooling gas is contacted with mixed gas, 4-cyanopyridine is separated out, slurry formed by the 4-cyanopyridine and cooling water is discharged from a liquid outlet at the bottom of a spray tower 6, the slurry discharged from a liquid outlet at the bottom of the spray tower 6 enters a 4-cyanopyridine crude product obtained by centrifugation in a first centrifugal machine, the 4-cyanopyridine crude product discharged from a discharge port of the first centrifugal machine 7 enters a crystallization kettle 8 from a feed inlet above the crystallization kettle 8, ethanol or ether solvent is added from a solvent inlet at the right side of the top of the crystallization kettle 8 after heating and decoloring, the mixture is stirred until the 4-cyanopyridine is easily saturated, the temperature is reduced at a certain speed to separate out the 4-cyanopyridine in a 4-cyanopyridine saturated solution, and the 4-cyanopyridine is separated out and then discharged from a discharge port below the crystallization kettle 8 to enter a second centrifugal machine 9 to obtain a 4-cyanopyridine.
In the description herein, references to the description of "one embodiment," "an example," "a specific example," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the present invention disclosed above are intended only to help illustrate the present invention. The preferred embodiments are not exhaustive and do not limit the specific implementations of the invention. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and its practical applications, to thereby enable others skilled in the art to best understand the invention for and utilize the invention. The present invention is limited only by the claims and their full scope and equivalents.
Claims (6)
1. An apparatus for synthesizing 4-cyanopyridine, comprising: the device comprises a first vaporizer (1), a second vaporizer (2), a mixer (3), an air pump (4), a fixed bed reactor (5), a spray tower (6), a first centrifuge (7), a crystallization kettle (8) and a second centrifuge (9), wherein an air outlet at the upper side of the first vaporizer (1) is connected with an air inlet at the upper side of the mixer (3), an air outlet at the upper side of the second vaporizer (2) is connected with an air inlet at the upper side of the mixer (3), an air inlet at the upper side of the mixer (3) is connected with an air outlet of the air pump (4), an air outlet at the bottom of the mixer (3) is connected with a top feed inlet of the fixed bed reactor (5), a bottom discharge outlet of the fixed bed reactor (5) is connected with an air inlet below the left side of the spray tower (6), a liquid outlet at the bottom of the spray tower (6) is connected with a left feed inlet of the first centrifuge, a discharge hole at the bottom of the first centrifugal machine (7) is connected with a feed inlet above the crystallization kettle (8), and a discharge hole below the crystallization kettle (8) is connected with a feed inlet above the second centrifugal machine (9).
2. The apparatus for synthesizing 4-cyanopyridine according to claim 1, wherein: the heating system is characterized in that a snake-shaped vaporization pipe is arranged in the first vaporizer (1), the vaporization pipe is coated with a heating medium pipe, a heating medium inlet is formed in the right side of the first vaporizer (1), a heating medium outlet is formed in the left side of the first vaporizer (1), the second vaporizer (2) is identical to the first vaporizer (1) in structure, a liquid inlet of the first vaporizer (1) is externally connected with a 4-methylpyridine liquid storage tank, and a liquid inlet of the second vaporizer (2) is externally connected with a liquid ammonia liquid storage tank.
3. The apparatus for synthesizing 4-cyanopyridine according to claim 1, wherein: the top of the mixer (3) is provided with a first air inlet, a second air inlet and a third air inlet, and electromagnetic valves are arranged at the first air inlet, the second air inlet and the third air inlet.
4. The apparatus for synthesizing 4-cyanopyridine according to claim 1, wherein: fixed bed reactor (5) top is equipped with the top and is equipped with the distributor, the distributor is connected with the feed inlet at fixed bed reactor (5) top, with the inside catalyst fixed bed that is equipped with of fixed bed reactor (5), both ends are equipped with heat medium import and heat medium export respectively about fixed bed reactor (5) right side outer wall is equipped with, and fixed bed reactor (5) bottom is equipped with the discharge gate.
5. The apparatus for synthesizing 4-cyanopyridine according to claim 1, wherein: the spray tower is characterized in that a spray device is arranged at the top end of the spray tower (6), a cooling water inlet is formed in the top of the spray tower (6), the spray device is connected with the cooling water inlet, an air inlet is formed below the left side of the spray tower (6), an air outlet is formed above the right side of the spray tower (6), a liquid outlet is formed in the bottom of the spray tower (6), and a tail gas treatment device is externally connected with the air outlet of the spray tower (6).
6. The apparatus for synthesizing 4-cyanopyridine according to claim 1, wherein: the inside puddler that is equipped with in crystallization cauldron (8), the puddler is connected with the motor in the middle of crystallization cauldron (8) top, and crystallization cauldron (8) top left side is equipped with the feed inlet, and crystallization cauldron (8) top right side is equipped with the solvent import, and crystallization cauldron (8) outer wall is equipped with the cold and hot medium jacket layer, is equipped with the discharge gate in the middle of crystallization cauldron (8) bottom.
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| CN201921932600.6U CN211078991U (en) | 2019-11-11 | 2019-11-11 | Device for synthesizing 4-cyanopyridine |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113289557A (en) * | 2021-06-16 | 2021-08-24 | 武汉松石科技股份有限公司 | Organic matter fluorination gas-liquid reaction system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113289557A (en) * | 2021-06-16 | 2021-08-24 | 武汉松石科技股份有限公司 | Organic matter fluorination gas-liquid reaction system |
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