CN211964174U - Production device of 6-aminocapronitrile - Google Patents
Production device of 6-aminocapronitrile Download PDFInfo
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- CN211964174U CN211964174U CN202020447572.5U CN202020447572U CN211964174U CN 211964174 U CN211964174 U CN 211964174U CN 202020447572 U CN202020447572 U CN 202020447572U CN 211964174 U CN211964174 U CN 211964174U
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Abstract
The utility model relates to a production device of 6-aminocapronitrile, including first reation kettle, rectifying still, second reation kettle, first condensation reflux unit, vacuum unit, second condensation reflux unit, pressure balance pipe, first return flow control valve and first return flow control valve. The discharge hole of the first reaction kettle is connected with the feed inlet of the rectifying kettle; the discharge hole of the rectifying kettle is connected with the feed inlet of the second reaction kettle; the discharge hole of the second reaction kettle is connected with the other feed inlet of the rectifying kettle; two ends of the first condensation reflux device are connected with the first reaction kettle and the first reflux control valve; the vacuum unit is connected with the rectifying kettle; two ends of the second condensation reflux device are connected with the second reaction kettle and the pressure balance pipe; two ends of the pressure balance pipe are connected with the second reaction kettle and the second condensation reflux device; the first reflux control valve is connected with the joint of the second condensation reflux device and the pressure balancing pipe. The device has the advantages of high energy utilization rate, low energy consumption, high product yield, easy control and capability of simplifying actual production operation.
Description
Technical Field
The utility model relates to an industrial production device of amino nitrile products, in particular to an industrial production device of 6-amino capronitrile products.
Background
6-aminocapronitrile is an important intermediate for synthesizing chemical materials, is expensive, and can be hydrogenated to obtain a downstream product 1, 6-hexanediamine. The 1, 6-hexamethylene diamine is one of raw materials of three large nylons, can be used for producing products such as nylon 66, nylon 610, hexamethylene diisocyanate and the like, and further can be prepared into various nylon resins, nylon fibers, engineering plastics and other bulk goods. Currently, a caprolactam ammonolysis process is mostly adopted in industry to produce 6-aminocapronitrile products, the production process has very harsh conditions, reaction materials are generally required to be heated to a high temperature of more than 350 ℃, the requirements on the reliability of production equipment and production control are extremely high, the actual production operation is not facilitated, the production efficiency is low, the energy consumption is high, and the product yield is low.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the technical problem that a production device of 6-aminocapronitrile is provided, the utility model discloses a device operation is complicated, production efficiency is low in the device can solve 6-aminocapronitrile product industrial production, and the energy consumption is high, product yield low scheduling problem.
The utility model adopts the technical proposal that: a production device of 6-aminocapronitrile comprises a first reaction kettle, a rectifying kettle, a second reaction kettle, a first condensation reflux device, a vacuum unit, a second condensation reflux device, a pressure balance pipe, a first reflux control valve and a second reflux control valve;
the discharge hole of the first reaction kettle is connected with the first feed hole of the rectifying kettle; the discharge hole of the rectifying kettle is connected with the first feed hole of the second reaction kettle; the discharge hole of the second reaction kettle is connected with the second feed inlet of the rectifying kettle; two ends of the first condensation reflux device are respectively connected with the first reaction kettle and the first reflux control valve; the vacuum unit is connected with the rectifying kettle; two ends of the second condensation reflux device are respectively connected with the second reaction kettle and the pressure balance pipe; two ends of the pressure balance pipe are respectively connected with the second reaction kettle and the second condensation reflux device; and the second reflux control valve is connected with the joint of the second condensation reflux device and the pressure balance pipe.
The first reaction kettle is a reaction kettle with a coil pipe and a stirring device; the rectifying kettle is a reaction kettle with a coil pipe and a rectifying device; the second reaction kettle is a reaction kettle with a coil pipe and a stirring device.
The coil pipes are all connected in series; the coil is made of one or more of 309 stainless steel, SS316 stainless steel, 408 stainless steel, nickel-molybdenum alloy or titanium-molybdenum alloy.
The coil pipe is connected with the kettle wall of the first reaction kettle through a flange without adopting direct welding, so that the side pipe is convenient to disassemble, assemble and maintain, the top and the bottom of the coil pipe are separated from the kettle body height of 1/3 at two ends of the first reaction kettle, and the heat transfer rate is accelerated. The coil pipe is connected with the kettle wall of the second reaction kettle through a flange, so that the coil pipe is convenient to disassemble, assemble and maintain, the coil pipe is attached to the kettle wall in a snake-shaped mode, and the distance between the coil pipe and the kettle wall is about 5-8 cm, so that heat transfer is facilitated. The coil pipe is connected with the kettle wall of the rectifying kettle through a flange.
The stirring device is a straight blade opening turbine type stirrer, an inclined blade opening turbine type stirrer or a bent blade opening turbine type stirrer.
The rectifying device is a rectifying tower. The height of the rectifying tower is about 5-10 m, and the inner diameter is 0.5-1.0 m. The gas phase outlet of the rectifying tower is connected with a vacuum unit through an ethylene glycol refrigerating fluid heat exchanger with a refrigerant of-30 ℃, the gas phase at the top of the rectifying tower is condensed into a liquid phase, and the liquid phase is pumped out of a packaging area through a magnetic pump.
The rectifying tower is a packed tower.
The filler of the packed tower is a two-ring filler, a stepped ring filler, an arc saddle filler, a square saddle filler or a spherical filler.
The first condensation reflux device is a water-cooled condenser; the vacuum unit is a rotary vane vacuum pump; the second condensation reflux device is a vertical efficient heat exchanger; the pressure balance pipe is a tetrafluoro lining pipe or a 316L stainless steel pipe or a nickel-copper alloy pipe.
The first condensation reflux device is respectively connected with the first reaction kettle and the first reflux control valve through flanges, and the refrigerant is deep cold water with the temperature of 15 ℃ below zero, so that the reflux effect can be improved. The heat exchange medium of the second condensing and refluxing device is ethylene glycol aqueous solution, so that the heat exchange efficiency can be improved. The gas-liquid pressure balance pipe is respectively connected to the upper end of the second condensation reflux device and the bottom of the second reaction kettle through flanges.
The vacuum unit is a high-power oil-sealed vacuum pump, a condenser with a refrigerant as chilled water is arranged in the vacuum unit, and circulating liquid of the vacuum pump is ethylene glycol, so that non-condensable gas coming out from the top of the rectifying tower during operation can be well dissolved in the circulating liquid, and the later-stage circulating liquid can be conveniently recovered. The vacuum unit is connected to the top of the rectifying tower through a stainless steel pipeline lined with polytetrafluoroethylene, and the pipeline lined with polytetrafluoroethylene is used for preventing ammonia gas, low-boiling-point organic acid and the like from corroding.
The water-cooled condenser is a vertical shell-and-tube condenser or a sleeve-type condenser or a spiral plate condenser or a plate condenser; the rotary-vane vacuum pump is a slide valve type vacuum pump or a fixed-vane type vacuum pump or a trochoid type vacuum pump or a multi-chamber rotary-vane type vacuum pump; the vertical high-efficiency heat exchanger is a spiral plate type heat exchanger or a plate fin type heat exchanger or a heat pipe type heat exchanger.
The condensate flow path channels of the condenser and the heat exchanger are both designed with U-shaped bends to prevent the gas from mixing with the condensate.
The discharge hole of the first reaction kettle is connected with the first feed hole of the rectifying kettle through a pipeline with a first discharge valve; the discharge hole of the rectifying kettle is connected with the first feed hole of the second reaction kettle through a pipeline with a second discharge valve; and the discharge hole of the second reaction kettle is connected with the second feed inlet of the rectifying kettle through a pipeline with a third discharge valve.
The utility model has the advantages that:
1. the heating coils of the first reaction kettle, the rectifying kettle and the second reaction kettle are all connected in series, so that the heat energy utilization rate can be improved.
2. First reation kettle and second reation kettle all make the cauldron in the pressure boost through adjusting the backward flow control valve to the mode ejection of compact with the material extrusion in the cauldron, such ejection of compact mode can the energy saving, reduces the energy consumption.
3. The second reaction kettle is connected with the pressure balance pipe, so that redundant ammonia gas generated in the reaction process can enter from the kettle bottom to participate in the reaction again, and the product yield can be improved.
4. The pipeline device has simple and clear connection mode, is easy to control and is beneficial to simplifying the actual production operation.
Drawings
FIG. 1 is a diagram showing the layout of a 6-aminocapronitrile production apparatus.
In the figure: the device comprises a first reaction kettle 1, a rectifying kettle 2, a second reaction kettle 3, a first condensation reflux device 4, a vacuum unit 5, a second condensation reflux device 6, a pressure balance pipe 7, a first reflux control valve 8, a second reflux control valve 9, a first discharge valve 10, a second discharge valve 11, a third discharge valve 12, a second reaction kettle feed inlet 13, a steam inlet 14, a fourth discharge valve 15, a steam outlet valve 16 and a first reaction kettle feed inlet 17.
Detailed Description
The present invention will be further explained with reference to the accompanying drawings.
As shown in fig. 1, a 6-aminocapronitrile production apparatus comprises a first reaction vessel 1, a rectifying vessel 2, a second reaction vessel 3, a first condensing reflux device 4, a vacuum unit 5, a second condensing reflux device 6, a pressure balance pipe 7, a first reflux control valve 8 and a first reflux control valve 9;
the discharge hole of the first reaction kettle 1 is connected with the first feed hole of the rectifying kettle 2; the discharge hole of the rectifying kettle 2 is connected with the first feed hole of the second reaction kettle 3; the discharge hole of the second reaction kettle 3 is connected with the second feed inlet of the rectifying kettle 2; two ends of the first condensation reflux device 4 are respectively connected with the first reaction kettle 1 and the first reflux control valve 8; the vacuum unit 5 is connected with the rectifying still 2; two ends of the second condensation reflux device 4 are respectively connected with the second reaction kettle 3 and the pressure balance pipe 7; two ends of the pressure balance pipe 7 are respectively connected with the second reaction kettle 3 and the second condensation reflux device 4; the second return flow control valve 9 is connected with the joint of the second condensing and returning device 6 and the pressure balancing pipe 7.
Preferably, the first reaction kettle 1 is a reaction kettle with a coil pipe and a stirring device; the rectifying kettle 2 is a reaction kettle with a coil pipe and a rectifying device; the second reaction kettle 3 is a reaction kettle with a coil pipe and a stirring device.
Preferably, the coils are all connected in series; the coil is made of one or more of 309 stainless steel, SS316 stainless steel, 408 stainless steel nickel-molybdenum alloy or titanium-molybdenum alloy.
Preferably, the stirring device is a straight blade opening turbine type stirrer, an inclined blade opening turbine type stirrer or a bent blade opening turbine type stirrer. A gap is reserved between the stirring blade of the stirring device and the kettle body, the gap is 15-20 cm, and materials are conveniently mixed, conveyed and heat is conveniently transferred.
Preferably, the rectification device is a rectification column.
Preferably, the rectifying tower is a packed tower.
Preferably, the packing of the packed tower is two-ring packing or step ring packing or arc saddle packing or intalox saddle packing or spherical packing.
Preferably, the first condensing and refluxing device 4 is a water-cooled condenser; the vacuum unit 5 is a rotary vane vacuum pump; the first condensation reflux device 6 is a vertical efficient heat exchanger; the pressure balance pipe 7 is a tetrafluoro-lined pipe, a 316L stainless steel pipe or a nickel-copper alloy pipe.
Preferably, the water-cooled condenser is a vertical shell-and-tube condenser or a double-pipe condenser or a spiral plate condenser or a plate condenser; the rotary-vane vacuum pump is a slide valve type vacuum pump or a fixed-vane type vacuum pump or a trochoid type vacuum pump or a multi-chamber rotary-vane type vacuum pump; the vertical high-efficiency heat exchanger is a spiral plate type heat exchanger or a plate fin type heat exchanger or a heat pipe type heat exchanger.
Preferably, the discharge hole of the first reaction kettle 1 is connected with the first feed inlet of the rectifying kettle 2 through a pipeline with a first discharge valve 10; the discharge hole of the rectifying still 2 is connected with the first feed hole of the second reaction kettle 3 through a pipeline with a second discharge valve 11; and the discharge hole of the second reaction kettle 3 is connected with the second feed inlet of the rectifying kettle 2 through a pipeline with a third discharge valve 12.
The present invention relates to a 6-aminocapronitrile production apparatus as described in the following examples.
The implementation process is as follows:
after the first reaction kettle 1 is filled with the raw materials, the feeding valve is closed, the coil pipe is opened, steam is heated, and meanwhile, the stirring device is started. After the material temperature reaches the preset temperature, the first reflux control valve 4 is opened to a certain degree, the spiral plate type condenser 4 is adjusted to control the reflux size, and after the reflux reaction is carried out for a period of time, the first discharge valve 10 is opened to discharge the material to the rectifying still 2. When the liquid level of the rectifying still 2 reaches 1/3, opening the coil pipe for steam heating, simultaneously opening the slide valve type vacuum pump 5, and vacuumizing until the vacuum degree is more than-0.09 MPa. When the temperature in the rectifying still 2 reaches 60 ℃, low-boiling condensate, namely 6-aminocaproate product, can be seen. After the content of the 6-aminocaproate product is detected to be qualified, opening a second discharge valve 11, discharging to a second reaction kettle 3, and simultaneously adding reaction raw materials into the second reaction kettle 3 from a feed inlet 13. After the raw materials are fully filled, the feeding valve is closed, the coil pipe is opened, steam is heated, and meanwhile, the stirring device is started. And after the temperature of the material reaches a preset temperature, opening the second reflux control valve 9 to a certain degree, adjusting the plate-fin heat exchanger 6 to control the reflux size, and adjusting the pressure balance pipe 7 to control the ammonia gas emission amount. After reacting for a period of time, opening the third discharge valve 12 and discharging to the rectifying still 2, rectifying and purifying to obtain 6-aminocapronitrile at the bottom of the rectifying still, and discharging through the fourth discharge valve 15. Sampling and analyzing, wherein the product purity is 98.5%, the product quality requirement is met, and the product yield is 85.1%.
The above embodiments are merely preferred technical solutions of the present invention, and should not be considered as limitations of the present invention, and the features in the embodiments and the examples in the present application may be arbitrarily combined with each other without conflict. The protection scope of the present invention shall be defined by the claims and the technical solutions described in the claims, including the technical features of the equivalent alternatives as the protection scope. Namely, equivalent alterations and modifications within the scope of the invention are also within the scope of the invention.
Claims (10)
1. A production device of 6-aminocapronitrile is characterized in that: the device comprises a first reaction kettle (1), a rectifying kettle (2), a second reaction kettle (3), a first condensation reflux device (4), a vacuum unit (5), a second condensation reflux device (6), a pressure balance pipe (7), a first reflux control valve (8) and a second reflux control valve (9);
the discharge hole of the first reaction kettle (1) is connected with the first feed hole of the rectifying kettle (2); the discharge hole of the rectifying kettle (2) is connected with the first feed hole of the second reaction kettle (3); the discharge hole of the second reaction kettle (3) is connected with the second feed hole of the rectifying kettle (2); two ends of the first condensation reflux device (4) are respectively connected with the first reaction kettle (1) and the first reflux control valve (8); the vacuum unit (5) is connected with the rectifying still (2); two ends of the second condensation reflux device (6) are respectively connected with the second reaction kettle (3) and the pressure balance pipe (7); two ends of the pressure balance pipe (7) are respectively connected with the second reaction kettle (3) and the second condensation reflux device (6); and the second reflux control valve (9) is connected with the joint of the second condensation reflux device (6) and the pressure balance pipe (7).
2. The apparatus for producing 6-aminocapronitrile according to claim 1, wherein: the first reaction kettle (1) is a reaction kettle with a coil pipe and a stirring device; the rectifying kettle (2) is a reaction kettle with a coil pipe and a rectifying device; the second reaction kettle (3) is a reaction kettle with a coil pipe and a stirring device.
3. The apparatus for producing 6-aminocapronitrile according to claim 2, wherein: the coil pipes are all connected in series; the coil is made of one or more of 309 stainless steel, SS316 stainless steel, 408 stainless steel, nickel-molybdenum alloy or titanium-molybdenum alloy.
4. The apparatus for producing 6-aminocapronitrile according to claim 2, wherein: the stirring device is a straight blade opening turbine type stirrer, an inclined blade opening turbine type stirrer or a bent blade opening turbine type stirrer.
5. The apparatus for producing 6-aminocapronitrile according to claim 2, wherein: the rectifying device is a rectifying tower.
6. The apparatus for producing 6-aminocapronitrile according to claim 5, wherein: the rectifying tower is a packed tower.
7. The apparatus for producing 6-aminocapronitrile according to claim 6, wherein: the filler of the packed tower is a two-ring filler, a stepped ring filler, an arc saddle filler, a square saddle filler or a spherical filler.
8. The apparatus for producing 6-aminocapronitrile according to claim 1, wherein: the first condensation reflux device (4) is a water-cooled condenser; the vacuum unit (5) is a rotary vane vacuum pump; the second condensation reflux device (6) is a vertical efficient heat exchanger; the pressure balance pipe (7) is a tetrafluoro-lined pipe or a 316L stainless steel pipe or a nickel-copper alloy pipe.
9. The apparatus for producing 6-aminocapronitrile according to claim 8, wherein: the water-cooled condenser is a vertical shell-and-tube condenser or a sleeve-type condenser or a spiral plate condenser or a plate condenser; the rotary-vane vacuum pump is a slide valve type vacuum pump or a fixed-vane type vacuum pump or a trochoid type vacuum pump or a multi-chamber rotary-vane type vacuum pump; the vertical high-efficiency heat exchanger is a spiral plate type heat exchanger or a plate fin type heat exchanger or a heat pipe type heat exchanger.
10. The apparatus for producing 6-aminocapronitrile according to claim 1, wherein: the discharge hole of the first reaction kettle (1) is connected with the first feed hole of the rectifying kettle (2) through a pipeline with a first discharge valve (10); the discharge hole of the rectifying kettle (2) is connected with the first feed hole of the second reaction kettle (3) through a pipeline with a second discharge valve (11); and the discharge hole of the second reaction kettle (3) is connected with the second feed inlet of the rectifying kettle (2) through a pipeline with a third discharge valve (12).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020447572.5U CN211964174U (en) | 2020-03-31 | 2020-03-31 | Production device of 6-aminocapronitrile |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020447572.5U CN211964174U (en) | 2020-03-31 | 2020-03-31 | Production device of 6-aminocapronitrile |
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| Publication Number | Publication Date |
|---|---|
| CN211964174U true CN211964174U (en) | 2020-11-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202020447572.5U Active CN211964174U (en) | 2020-03-31 | 2020-03-31 | Production device of 6-aminocapronitrile |
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| CN (1) | CN211964174U (en) |
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- 2020-03-31 CN CN202020447572.5U patent/CN211964174U/en active Active
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