CN211611688U - 4-cyanopyridine's crystallization purification device - Google Patents
4-cyanopyridine's crystallization purification device Download PDFInfo
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- CN211611688U CN211611688U CN201921932602.5U CN201921932602U CN211611688U CN 211611688 U CN211611688 U CN 211611688U CN 201921932602 U CN201921932602 U CN 201921932602U CN 211611688 U CN211611688 U CN 211611688U
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Abstract
The utility model provides a 4-cyanopyridine's crystallization purification device, the device comprises a device body, inside crystallization case and the separator box of being equipped with of device body, crystallization case fixed mounting is in the separator box top, separator box bottom fixed mounting base, the inside hollow shaft that is equipped with of crystallization incasement portion, hollow shaft lower extreme fixed mounting puddler, the inside cold heat medium pipe that all is equipped with of hollow shaft and puddler, the inside centrifugal basket that is equipped with of separator box, centrifugal basket bottom is connected with the sealed rotation of separator box, the discharge gate has been seted up to centrifugal basket bottom, centrifugal basket lateral wall is equipped with the screen cloth, the fixed middle installation of separator box bottom goes out the hopper, the discharge gate communicates with each other with. The utility model discloses 4-cyanopyridine purification device, rational in infrastructure, easy operation can separate 3-cyanopyridine and 4-cyanopyridine, has improved 4-cyanopyridine purity and extraction rate, is fit for with industrial production usefulness.
Description
Technical Field
The utility model relates to a chemical industry equipment technical field, in particular to 4-cyanopyridine's crystallization purification device.
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. 4-cyanopyridine is mainly derived from ammoxidation synthesis of alkylpyridine, but 4-cyanopyridine is usually generated by using alkylpyridine, and in order to obtain a required high-purity intermediate raw material, a crude product of 4-cyanopyridine must be separated and purified, but 3-cyanopyridine is an isomer of 4-cyanopyridine, the boiling points of 3-cyanopyridine and 4-cyanopyridine are only different by 5 ℃, and separation is difficult, and at present, a vacuum rectification method is mostly adopted for industrial separation.
3-cyanopyridine and 4-cyanopyridine are easy sublimating substances, a small amount of byproduct fumaric dinitrile exists in the mixture, the fumaric dinitrile is easy to generate polymerization reaction in the rectification separation process, and the rectification device equipment is easy to block to influence the normal operation of the fumaric dinitrile, so that the separation effect of the 4-cyanopyridine in the industrial production is poor, and the operation cost is high. Therefore, a device for separating and purifying 4-cyanopyridine is needed to meet the requirement of industrial production.
SUMMERY OF THE UTILITY MODEL
Aiming at the defects of the prior art, the utility model provides a 4-cyanopyridine's crystallization purification device, rational in infrastructure, easy operation can separate 3-cyanopyridine and 4-cyanopyridine, has improved 4-cyanopyridine purity.
The utility model provides a 4-cyanopyridine crystallization purification device, which comprises a device body, wherein a crystallization box and a separation box are arranged inside the device body, the crystallization box is fixedly arranged above the separation box, a base is fixedly arranged at the bottom of the separation box, a hollow shaft is arranged inside the crystallization box, a stirring rod is fixedly arranged at the lower end of the hollow shaft, the upper end of the hollow shaft penetrates through the middle of the top of the crystallization box, the hollow shaft is connected with the crystallization box in a sealing and rotating way, a rotary joint is fixedly arranged at the top end of the hollow shaft, a gear is fixedly arranged on the surface of the hollow shaft between the crystallization box and the rotary joint, a first motor is fixedly arranged at the top of the crystallization box, a gear is arranged on an output shaft of the first motor, the gear on the hollow shaft is meshed with the gear on the output shaft of the first motor, the blanking port is communicated with the inside of the separation box, the inside centrifugal basket that is equipped with of separation box, the centrifugation basket bottom is connected with the sealed rotation of separation box, be equipped with the column spinner in the middle of the centrifugation basket, the inside fixed mounting axis of rotation of column spinner, the axis of rotation top is fixed with the column spinner, axis of rotation bottom fixed mounting belt pulley, the discharge gate has been seted up to the centrifugation basket bottom, the fixed middle hopper of installing of separation box bottom, the discharge gate communicates with each other with a hopper, separation box bottom left side fixed mounting motor two, fixed mounting belt pulley on the output shaft of motor two, the output shaft and the axis of rotation of motor two pass through the belt and are connected.
Further preferably, cooling and heating medium pipes are arranged inside the hollow shaft and the stirring rod, the cooling and heating medium pipes in the hollow shaft are communicated with the cooling and heating medium pipes in the stirring rod, the rotary joint is a double-channel liquid rotary joint, a cooling and heating medium inlet and a cooling and heating medium outlet are formed in the rotary joint, and a water inlet end and a water outlet end of the cooling and heating medium pipes in the hollow shaft are respectively connected with the cooling and heating medium inlet and the cooling and heating medium outlet in the rotary joint.
Further preferably, a cooling and heating medium pipe is arranged inside the heating layer, and the cooling and heating medium pipe inside the heating layer is annularly wound on the outer wall of the crystallization box.
Further preferably, the side wall of the centrifugal basket is provided with a screen, and the top end of the rotary column is provided with an obliquely arranged material-homogenizing plate.
Further preferably, electric valves are arranged at the blanking port and the discharging port.
Compared with the prior art, the utility model has the advantages that:
the utility model discloses the inside cold and hot medium pipe that all is equipped with of hollow shaft and puddler can heat or cool down the solution or powder in the crystallization case in the stirring process, combines the zone of heating of crystallization case outer wall cladding to heat or cool down the solution or powder in the crystallization case jointly, and heating or cooling effect is good, can the speed of accurate control intensification or cooling to control 4-cyanopyridine crystal to appear, improve the purity of 4-cyanopyridine; the utility model discloses crystallization bottom of the case portion fixed mounting separator box, the inside centrifugation basket that is equipped with of separator box, 4-cyanopyridine crystal are separated out and are accomplished crystal and solvent separation by centrifugation rapidly after forming the thick liquids, prevent that 4-cyanopyridine from dissolving once more, have improved the extraction rate of 4-cyanopyridine. To sum up, the utility model discloses 4-cyanopyridine purification device, rational in infrastructure, easy operation can separate 3-cyanopyridine and 4-cyanopyridine, has improved 4-cyanopyridine purity and extraction rate, is fit for with industrial production usefulness.
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 view of the centrifugal screen of the present invention.
In the figure:
1-device body, 2-crystallization box, 3-separation box, 4-base, 5-hollow shaft, 6-stirring rod, 7-rotary joint, 8-motor I, 9-feed inlet, 10-water inlet, 11-heating layer, 12-blanking port, 13-centrifugal basket, 14-rotary column, 15-rotary shaft, 16-discharge port, 17-discharge hopper, 18-motor II and 19-water outlet.
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 figure 1-2, a 4-cyanopyridine crystallization purification device comprises a device body 1, a crystallization box 2 and a separation box 3 are arranged in the device body 1, the crystallization box 2 is fixedly arranged above the separation box 3, a base 4 is fixedly arranged at the bottom of the separation box 3, a hollow shaft 5 is arranged in the crystallization box 2, a stirring rod 6 is fixedly arranged at the lower end of the hollow shaft 5, the upper end of the hollow shaft 5 penetrates through the middle of the top of the crystallization box 2, the hollow shaft 5 is in sealed and rotary connection with the crystallization box 2, a rotary joint 7 is fixedly arranged at the top end of the hollow shaft 5, a gear is fixedly arranged on the surface of the hollow shaft 5 between the crystallization box 2 and the rotary joint 7, a motor I8 is fixedly arranged at the top of the crystallization box 2, a gear is arranged on an output shaft of the motor I8, the gear on the hollow shaft 5 is meshed with the gear on the output, the outer wall of the crystallization box 2 is coated with a heating layer 11, a blanking port 12 is formed in the bottom of the crystallization box 2, the blanking port 12 is communicated with the inside of the separation box 3, a centrifugal basket 13 is arranged inside the separation box 3, the bottom of the centrifugal basket 13 is connected with the separation box 3 in a sealing and rotating mode, a rotary column 14 is arranged in the middle of the centrifugal basket 13, a rotary shaft 15 is fixedly installed inside the rotary column 14, the top end of the rotary shaft 15 is fixed with the rotary column 14, a belt pulley is fixedly installed at the bottom end of the rotary shaft 15, a discharging port 16 is formed in the bottom of the centrifugal basket 13, a discharging hopper 17 is installed in the middle of the bottom of the separation box 3, the discharging port 16 is communicated with the discharging hopper 17, a motor II 18 is fixedly installed on the left side of the bottom of the separation box.
A cooling and heating medium pipe is arranged inside the heating layer 11, and the cooling and heating medium pipe inside the heating layer 11 is annularly wound on the outer wall of the crystallization box.
The side wall of the centrifugal basket 13 is provided with a screen, and the top end of the rotary column 14 is provided with a conical material-homogenizing plate.
Electric valves are arranged at the blanking port 12 and the discharge port 16.
The working principle is as follows:
the inside hollow shaft 5 that is equipped with of crystallization case 2, 5 lower extreme fixed mounting puddler 6 of hollow shaft, 5 top fixed mounting rotary joint 7 of hollow shaft, hollow shaft 5 and puddler 6 are inside all to be equipped with the heating medium pipe, the heating medium pipe in the hollow shaft 5 communicates with each other with the cold and hot medium pipe in the puddler 6, refrigerant or heat medium are from getting into hollow shaft 5 and puddler 6 through rotary joint 7, can heat or cool down solution or powder in crystallization case 2 at the stirring in-process, combine the zone of heating of 2 outer wall cladding of crystallization case 11 to solution or powder heating or cooling in crystallization case 2 jointly, it is effectual to heat or cool down, it is even stable to heat or cool down.
When the device is used for purifying 4-cyanopyridine, crude 4-cyanopyridine is firstly put into a crystallization box 2 from a feed inlet 9, a motor I is started, heating medium is introduced into a hollow shaft 5 and a heating layer 11, the crude 4-cyanopyridine in the crystallization box 2 is heated while stirring, ethanol or diethyl ether is added from a water inlet 10 after heating and decoloring, the mixture is stirred until the 4-cyanopyridine is dissolved to form saturated solution, then refrigerant is introduced into the hollow shaft 5 and the heating layer 11, the cooling speed is controlled, the 4-cyanopyridine is separated out to form slurry containing mixed 4-cyanopyridine crystals and ethanol or diethyl ether, a valve at a blanking port 12 is opened, the mixed slurry falls into a centrifugal basket 13 in a separation box 3, a motor II is started, the centrifugal basket 13 rotates at high speed, the ethanol or diethyl ether in the slurry enters the separation box 3 from a screen at the side wall of the centrifugal screen, and 4-cyanopyridine crystals in the slurry are left in the centrifugal basket 13, and finally the 4-cyanopyridine crystals are discharged from a discharge port 16 and dried to obtain a pure 4-cyanopyridine product.
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 (5)
1. A4-cyanopyridine crystallization purification device is characterized in that: comprises a device body (1), a crystallization box (2) and a separation box (3) are arranged inside the device body (1), the crystallization box (2) is fixedly arranged above the separation box (3), a base (4) is fixedly arranged at the bottom of the separation box (3), a hollow shaft (5) is arranged inside the crystallization box (2), a stirring rod (6) is fixedly arranged at the lower end of the hollow shaft (5), the upper end of the hollow shaft (5) penetrates through the middle of the top of the crystallization box (2), the hollow shaft (5) is in sealed rotating connection with the crystallization box (2), a rotary joint (7) is fixedly arranged at the top end of the hollow shaft (5), a gear is fixedly arranged on the surface of the hollow shaft (5) between the crystallization box (2) and the rotary joint (7), a motor I (8) is fixedly arranged at the top of the crystallization box (2), a gear is arranged on an output shaft of the motor I (8), and is meshed with the gear on the, the left side of the top of the crystallization box (2) is provided with a feeding hole (9), the right side of the top of the crystallization box (2) is provided with a water inlet (10), the outer wall of the crystallization box (2) is coated with a heating layer (11), the bottom of the crystallization box (2) is provided with a blanking hole (12), the blanking hole (12) is communicated with the inside of the separation box (3), the inside of the separation box (3) is provided with a centrifugal basket (13), the bottom of the centrifugal basket (13) is rotationally connected with the separation box (3) in a sealing way, a rotary column (14) is arranged in the middle of the centrifugal basket (13), a rotary shaft (15) is fixedly arranged in the rotary column (14), the top end of the rotary shaft (15) is fixed with the rotary column (14), the bottom of the rotary shaft (15) is fixedly provided with a belt pulley, the bottom of the centrifugal basket (13) is provided with a discharging hole (16, a second motor (18) is fixedly installed on the left side of the bottom of the separation box (3), a belt pulley is fixedly installed on an output shaft of the second motor (18), the output shaft of the second motor (18) is connected with the rotating shaft (15) through a belt, and a water outlet (19) is formed in the right side of the bottom of the separation box (3).
2. The apparatus for purifying crystallization of 4-cyanopyridine according to claim 1, wherein: hollow shaft (5) and puddler (6) inside all are equipped with the heating medium pipe, and the heating medium pipe in hollow shaft (5) communicates with each other with the heating medium pipe in puddler (6), and rotary joint (7) are binary channels liquid rotary joint, are equipped with cold and hot media import and cold and hot media export on rotary joint (7), and the heating medium pipe in hollow shaft (5) is intake end and water outlet end respectively with the cold and hot media import and the cold and hot media exit linkage on rotary joint (7).
3. The apparatus for purifying crystallization of 4-cyanopyridine according to claim 1, wherein: heating layer (11) inside is equipped with cold and hot medium pipe, and the cold and hot medium pipe ring winding of heating layer (11) inside sets up at crystallization case outer wall.
4. The apparatus for purifying crystallization of 4-cyanopyridine according to claim 1, wherein: the side wall of the centrifugal basket (13) is provided with a screen, and the top end of the rotary column (14) is provided with a conical material-homogenizing plate.
5. The apparatus for purifying crystallization of 4-cyanopyridine according to claim 1, wherein: electric valves are arranged at the blanking port (12) and the discharge port (16).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921932602.5U CN211611688U (en) | 2019-11-11 | 2019-11-11 | 4-cyanopyridine's crystallization purification device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201921932602.5U CN211611688U (en) | 2019-11-11 | 2019-11-11 | 4-cyanopyridine's crystallization purification device |
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| CN211611688U true CN211611688U (en) | 2020-10-02 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110746352A (en) * | 2019-11-11 | 2020-02-04 | 安徽瑞邦生物科技有限公司 | Method for separating 4-cyanopyridine by solvent cooling crystallization |
| CN112619575A (en) * | 2020-10-13 | 2021-04-09 | 峨眉山宏昇药业股份有限公司 | Medicine intermediate preparation facilities |
| CN113717244A (en) * | 2021-09-07 | 2021-11-30 | 福州帅宝生物科技有限公司 | Purification device for preparing composite polypeptide material and processing method thereof |
-
2019
- 2019-11-11 CN CN201921932602.5U patent/CN211611688U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110746352A (en) * | 2019-11-11 | 2020-02-04 | 安徽瑞邦生物科技有限公司 | Method for separating 4-cyanopyridine by solvent cooling crystallization |
| CN110746352B (en) * | 2019-11-11 | 2023-03-14 | 安徽瑞邦生物科技有限公司 | Method for separating 4-cyanopyridine by solvent cooling crystallization |
| CN112619575A (en) * | 2020-10-13 | 2021-04-09 | 峨眉山宏昇药业股份有限公司 | Medicine intermediate preparation facilities |
| CN113717244A (en) * | 2021-09-07 | 2021-11-30 | 福州帅宝生物科技有限公司 | Purification device for preparing composite polypeptide material and processing method thereof |
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