CN215162265U

CN215162265U - 2-hexanetriamine production system

Info

Publication number: CN215162265U
Application number: CN202120788866.9U
Authority: CN
Inventors: 陈恩之; 陈东生; 李宁; 张银杏; 张楠; 张传礼
Original assignee: Chongqing Huafeng New Material Research Institute Co ltd; Chongqing Huafeng Polyamide Co ltd; CHONGQING HUAFON CHEMICAL CO LTD
Current assignee: Chongqing Huafeng New Material Research Institute Co ltd; Chongqing Huafeng Polyamide Co ltd; CHONGQING HUAFON CHEMICAL CO LTD
Priority date: 2021-04-15
Filing date: 2021-04-15
Publication date: 2021-12-14
Anticipated expiration: 2031-04-15

Abstract

The utility model relates to a 2-hexanetriamine's production system, including solid-liquid separation equipment, dehydration tower, take off light tower, centrifuge, first refined tower, second refined tower, solid-liquid separation equipment's material import is used for linking to each other with reactor exhaust through gas-liquid separation, catalyst filtration, dealcoholize's mixture material source, and solid-liquid separation equipment passes through the overflow pipe to the dehydration tower feed, the bottom discharge gate of dehydration tower is to taking off light tower feed through the second pipeline, the bottom discharge gate of taking off light tower is to the centrifuge feed through the third pipeline, and this centrifuge's clear liquid export is to first refined tower feed through the fourth pipeline, the bottom discharge gate of first refined tower is to the refined tower feed of second through the fifth pipeline, the top discharge gate of second refined tower connects the condenser, to outer discharge target product. The utility model discloses simple structure, convenient operation can stably produce 2-hexanetriamine product in succession, satisfy chemical enterprise's actual demand.

Description

2-hexanetriamine production system

Technical Field

The utility model relates to a chemical industry field, in particular to 2-hexanetriamine's production system.

Background

2-hexanetriamine is a chemical substance with the chemical formula C₁₂H₂₉N₃Molecular weight 215.38, also known as dihexyltriamine, bis (hexamethylene) triamine, N- (6-aminohexyl) -1, 6-hexanediamine.

The 2-hexamethylene triamine can be used for replacing hexamethylene diamine and derivatives to produce epoxy resin curing agents, can also be used for synthesizing bis-1, 6 hexamethylene triamine pentamethylene phosphate serving as a scale inhibitor, and can also be used for spinning, papermaking auxiliaries, asphalt anti-stripping agents and the like.

However, at present, 2-hexanetriamine is usually obtained by purifying a byproduct obtained in a process for synthesizing hexamethylenediamine, and the 2-hexanetriamine has more impurities, low content and low overall value and cannot be sold as a product.

Disclosure of Invention

The utility model aims at the not enough of prior art, provide a production system of 2-hexanetriamine, its simple structure, convenient operation can stably produce 2-hexanetriamine product in succession, satisfy chemical enterprise's actual demand.

Realize the technical scheme of the utility model is that: the utility model provides a 2-hexanetriamine's production system, includes solid-liquid separation equipment, dehydration tower, takes off light tower, centrifuge, first refined tower, the refined tower of second, solid-liquid separation equipment's material import is used for linking to each other with reactor exhaust mixture material source through gas-liquid separation, catalyst filtration, dealcoholization, and solid-liquid separation equipment passes through the overflow pipe to the dehydration tower feed, the discharge gate at the bottom of the tower of dehydration tower is to taking off light tower feed through the second pipeline, the discharge gate at the bottom of the tower of taking off light tower is to centrifuge feed through the third pipeline, and this centrifuge's clear liquid export is to first refined tower feed through the fourth pipeline, the discharge gate at the bottom of the tower of first refined tower feeds to the refined tower of second through the fifth pipeline, the top discharge gate of the refined tower of second connects the condenser, to outer discharge target product.

Still include reactor, filter, dealcoholize tower, the bottom of reactor sets up the raw materials import, and the top of reactor sets up row material export, through gas-liquid separation device, links to each other with the import of filter, the export of filter is through first pipeline to the dealcoholize tower feed, is equipped with dealcoholize charge-in pump on this first pipeline, the bin outlet links to each other with solid-liquid separation device's material import at the bottom of the tower of dealcoholize tower.

The reactor is provided with a first cooler which is a coil or a jacket.

The gas-liquid separation device comprises a buffer tank and a flash tank, wherein the upper part of the buffer tank is connected with a discharge outlet of the reactor, an outlet at the top of the buffer tank is connected with the flash tank through a compressor and used for providing compressed hydrogen for the reactor, an outlet at the bottom of the buffer tank is connected with the flash tank through a sixth pipeline, a valve is arranged on the sixth pipeline, and an outlet at the bottom of the flash tank is connected with an inlet of a filter.

A filter feeding tank is arranged between the gas-liquid separation device and the filter, the filter feeding tank is provided with a second cooler which is a coil or a jacket, and a stirrer is arranged in the filter feeding tank.

The solid-liquid separation device comprises a third cooler and a decanter, wherein the upstream end of a material medium channel of the third cooler is used for being connected with a mixture source which is discharged by the reactor and is subjected to gas-liquid separation, catalyst filtration and dealcoholization, the downstream end of the material medium channel is connected with an inlet of the decanter, and the top of the decanter supplies materials to the dehydration tower through an overflow pipe.

The tower bottom discharge port of the dealcoholization tower is connected with the solid-liquid separation device through a heat medium channel of a heat exchanger, and the first pipeline passes through a cold medium channel of the heat exchanger to supply materials to the dealcoholization tower.

Adopt above-mentioned technical scheme to have following beneficial effect:

1. the utility model provides a 2-hexanetriamine's production system, utilize the reactor synthesis to obtain the mixture that uses 2-hexanetriamine as the owner, the mixture of formation is through gas-liquid separation, filter, dealcoholize, solid-liquid separation, the dehydration, take off lightly, and refine after the centrifugation, the content of 2-hexanetriamine reaches more than 90 wt% in the product that obtains, impurity organic matter content is less than 9 wt%, and water content control is below 1 wt%, and do not contain sodium hydroxide, can replace hexanediamine and derivative as the product and be used for producing the epoxy curing agent, also can be used to synthesize two 1 of scale inhibitor, 6 hexamethylene triamine pentamethylene phosphate, also can be used to weaving simultaneously, papermaking auxiliary agent, pitch antistripping agent etc.

2. The utility model discloses production system's gas-liquid separation device is located between reactor and the filter for with the excessive hydrogen separation and the recovery in the mixture that the reactor generated, guarantee the production safety of low reaches device, and reduce the manufacturing cost of enterprise. Gas-liquid separation includes buffer tank, flash tank, the upper portion of buffer tank with the row of the reactor material export links to each other, and the top export of buffer tank is through the compressor for provide compressed hydrogen to the reactor, and the bottom export of buffer tank passes through the sixth pipeline and links to each other with the flash tank, is equipped with the valve on the sixth pipeline, gets into the buffer tank from reactor exhaust mixture, and keeps temporarily, forms the liquid seal to excessive hydrogen, guarantees that excessive hydrogen is whole to be discharged from the top export of buffer tank, is used for recycle through the compressor compression, avoids excessive hydrogen to pass the buffer tank and gets into the low reaches and set up and cause the potential safety hazard. The tank bottom outlet of the flash tank is connected with the inlet of the filter, the high-temperature and high-pressure liquid phase temporarily retained in the buffer tank enters the flash tank, and after flash processing, the low-boiling-point impurities such as a very small amount of hydrogen and a small amount of ethanol which are mixed with the impurities are separated in a vapor state, and are condensed into a liquid state and then recycled.

3. The utility model discloses production system sets up the filter inlet pipe in the upper reaches of filter, and is equipped with second cooler and agitator, through agitator and second cooler cooperation, fully cools down to the reaction mixture, avoids the catalyst in the material to continue the catalysis to the reaction product, and then avoids generating the accessory substance, guarantees the yield of 2-hexanetriamine.

4. The solid-liquid separation device comprises a third cooler and a decanter, wherein a discharge outlet at the bottom of the dealcoholization tower is connected with an inlet of the decanter through the third cooler, the top of the decanter supplies materials to the dehydration tower through an overflow pipe, the temperature is reduced, the separation of sodium hydroxide in the reaction mixed liquid is facilitated, and the separation effect of the decanter can be effectively improved.

5. The tower bottom discharge port of the dealcoholization tower is connected with the solid-liquid separation device through a heat medium channel of a heat exchanger, the first pipeline passes through a cold medium channel of the heat exchanger to supply materials to the dealcoholization tower, and the materials entering the dealcoholization tower are preheated and heated by the materials discharged from the dealcoholization tower, so that the energy consumption of the dealcoholization tower is reduced, and the work load of a third cooler is reduced.

The following further description is made with reference to the accompanying drawings and detailed description.

Drawings

Fig. 1 is a schematic structural diagram of embodiment 1 of the present invention.

In the drawing, 1 is a reactor, 2 is a filter, 3 is a dealcoholization tower, 4 is a dehydration tower, 5 is a lightness-removing tower, 6 is a centrifuge, 7 is a gas-liquid separation device, 71 is a buffer tank, 72 is a flash tank, 8 is a dealcoholization feed pump, 9 is a solid-liquid separation device, 101 is a first refining tower, 102 is a second refining tower, 11 is a first cooler, 12 is a filter feed tank, 13 is a second cooler, 14 is a stirrer, 15 is a third cooler, 16 is a decanter, 17 is an overflow pipe, 18 is a heat exchanger, 19 is a condenser, 1a is a first pipeline, 1b is a second pipeline, 1c is a third pipeline, 1d is a fourth pipeline, and 1e is a fifth pipeline.

Detailed Description

The utility model discloses in, do not mark the equipment or the spare part of concrete structure, be the conventional equipment or spare part in chemical industry field usually, do not mark concrete connection mode, be the conventional connected mode in chemical industry field or the connected mode of producer suggestion usually. The used raw materials meet the requirements of relevant national or industrial standards.

Example 1

A production system of 2-hexanetriamine comprises a solid-liquid separation device 9, a dehydration tower 4, a lightness-removing tower 5, a centrifuge 6, a first refining tower 101 and a second refining tower 102. The material inlet of the solid-liquid separation device 9 is used for being connected with a mixture material source which is discharged by the reactor and is subjected to gas-liquid separation, catalyst filtration and dealcoholization, and the solid-liquid separation device 9 supplies materials to the dehydration tower 4 through an overflow pipe 17. The bin outlet at the bottom of dehydration tower 4 is to taking off light tower 5 feed through second pipeline 1b, the bin outlet at the bottom of taking off light tower 5 is to centrifuge 6 feed through third pipeline 1c, and this centrifuge 6's clear solution export is to first refining tower 101 feed through fourth pipeline 1d, and centrifuge 6's turbid liquid export is arranged to the scum tank for recycle. The bottom discharge port of the first refining tower 101 supplies materials to the second refining tower 102 through a fifth pipeline 1e, and the top discharge port of the second refining tower 102 is connected with a condenser 19 and discharges target products outwards.

Example 2

Referring to fig. 1, the production system of 2-hexanetriamine comprises a reactor 1, a filter 2, a dealcoholization tower 3, a dehydration tower 4, a light component removal tower 5 and a centrifuge 6. The bottom of the reactor 1 is provided with a raw material inlet, the top of the reactor is provided with a discharge outlet, and as the reaction is exothermic, a first cooler 11 is arranged in the reactor and used for eliminating reaction heat, specifically, the first cooler 11 is a coil or a jacket, and the reaction heat generated by the reactor is timely removed by using cooling water. The discharge outlet at the top of the reactor is connected with the inlet of the filter 2 through a gas-liquid separation device 7, which comprises a buffer tank 71 and a flash tank 72 in the embodiment, the upper part of the buffer tank 71 is connected with the discharge outlet of the reactor 1, the top outlet of the buffer tank 71 passes through a compressor (not shown), used for providing compressed hydrogen for the reactor 1, the bottom outlet of the buffer tank 71 is connected with the flash tank 72 through a fifth pipeline, a valve is arranged on the fifth pipeline, a condenser (not shown) is arranged at the outlet of the top of the flash tank 72, the outlet of the bottom of the flash tank 72 is connected with the inlet of the filter 2, and specifically, a filter feeding tank 12 is arranged between the outlet of the tank bottom of the flash tank and the filter, specifically, the outlet of the tank bottom of the flash tank is connected with the tank top of the filter feeding tank through a pipeline, and the tank bottom of the filter feeding tank is connected with the inlet of the filter through a pipeline. The filter feeding tank 12 is provided with a second cooler 13, the second cooler 13 is a coil or a jacket, the filter feeding tank 12 is provided with a stirrer 14 for cooling the gas-liquid separated material, and the filter is usually pressure-filtered by a filter screen with the specification of 1-20 μm, so that a filter feeding pump is further provided between the filter feeding tank and the filter. The outlet of the filter 2 supplies the material to the dealcoholization tower 3 through a first pipeline 1a, specifically, a dealcoholization feed tank is arranged between the filter and the dealcoholization tower, a dealcoholization feed pump 8 is arranged on the first pipeline 1a and is positioned at the downstream of the dealcoholization feed tank, the bottom discharge outlet of the dealcoholization tower 3 supplies the material to the dehydration tower 4 through a solid-liquid separation device 9, in this embodiment, the bottom discharge outlet of the dealcoholization tower 3 is connected with the solid-liquid separation device 9 through a heat medium channel of a heat exchanger 18, the first pipeline 1a passes through a cold medium channel of the heat exchanger 18 to supply the material to the dealcoholization tower 3, the solid-liquid separation device 9 comprises a third cooler 15 and a decanter 16, the third cooler is positioned at the downstream of the heat exchanger 18, the bottom discharge outlet of the dealcoholization tower 3 is connected with the inlet of the decanter 16 through the third cooler 15, the top of the decanter 16 supplies the material to the dehydration tower 4 through an overflow pipe 17, usually, set up material buffer tank between dewatering tower and decanter, the downstream end of overflow pipe links to each other with the tank deck of material buffer tank, sets up the dehydration charge-in pump between material buffer tank and the dewatering tower. The material is supplied to the lightness-removing column 5 from the bottom discharge outlet of the dehydration column 4 through a second pipeline 1 b. The bin outlet at the bottom of taking off light tower 5 is through the third pipeline 1c to the feed of centrifuge 6, this centrifuge 6's clear liquid export is through fourth pipeline 1d to the refined tower feed, in this embodiment, the quantity of refined tower is two, be first refined tower 101 respectively, second refined tower 102, centrifuge's clear liquid export is through fourth pipeline and first refined tower 101 feed, the bin outlet at the bottom of first refined tower is through the fifth pipeline to the refined tower feed of second, the condenser is connected to the top of the tower bin outlet of second refined tower for discharge target product, the bin outlet at the bottom of the second refined tower is used for linking to each other with burning device.

Example 3

A method for producing 2-hexanetriamine using the production system of example 2, comprising the steps of:

1) a premixed solution consisting of adiponitrile, an ethanol solution, a base and a catalyst and excessive hydrogen enter the reactor from a raw material inlet of the reactor. The weight ratio of adiponitrile, ethanol, catalyst and sodium hydroxide is 95: 45: 2: carrying out hydrogenation reaction at the temperature of 0.8 and 65-80 ℃ to obtain reaction mixed liquid;

2) separating excessive hydrogen from the reaction mixed liquid by a gas-liquid separation device, cooling the obtained liquid phase to 60 ℃, and filtering to obtain a reaction product;

3) the reaction product enters a dealcoholization tower, the temperature of the tower kettle is controlled to be 125 ℃, ethanol is removed until the content is less than 500ppm, and tower kettle liquid is discharged;

4) cooling the tower bottom liquid discharged in the step 3) to 75 ℃, allowing the tower bottom liquid to enter a solid-liquid separation device, separating sodium hydroxide from the tower bottom liquid, overflowing the obtained liquid phase to a dehydration tower, controlling the pressure at the top of the tower to be-85 KPaG, controlling the temperature of the tower bottom to be 125 ℃, removing water until the content of the water is less than 0.2 wt%, and discharging the tower bottom liquid;

5) the tower bottom liquid discharged in the step 4) enters a light component removal tower, the temperature of the tower bottom is controlled to be 130 ℃ under the condition of negative pressure of-92 KPaG, light components are removed, and the tower bottom liquid is discharged;

6) and 5) enabling the tower bottom liquid discharged in the step 5) to enter a centrifugal machine, adjusting the rotating speed of the centrifugal machine to 7000r/min according to material composition, simultaneously correspondingly adjusting the deslagging period to 45 min/time, discharging the separated turbid liquid from a liquid outlet, recycling, enabling the discharged clear liquid to enter a first refining tower, controlling the temperature of the tower bottom to be 135 ℃ under the condition of-95 KPaG, recovering hexamethylenediamine at the tower top, enabling the discharged tower bottom liquid to enter a second refining tower, controlling the temperature of the tower bottom to be 140 ℃ under the condition of-97 KPaG, and discharging at a condenser at the tower top of the second refining tower to obtain the target product.

Through detection, the content of the light component organic amine impurity 2-aminocyclopentylmethylamine in the product is 11ppm, the content of the target product 2-hexyltriamine is 95.26%, and the product does not contain sodium hydroxide.

Example 4

1) a premixed solution consisting of adiponitrile, an ethanol solution, a base and a catalyst and excessive hydrogen enter the reactor from a raw material inlet of the reactor. The weight ratio of adiponitrile, ethanol, catalyst and sodium hydroxide is 105: 55: 3: carrying out hydrogenation reaction at the temperature of 1.2 and 65-80 ℃ to obtain reaction mixed liquid;

2) separating excessive hydrogen from the reaction mixed liquid by a gas-liquid separation device, cooling the obtained liquid phase to 65 ℃, and filtering to obtain a reaction product;

3) the reaction product enters a dealcoholization tower, the temperature of the tower kettle is controlled to be 130 ℃, ethanol is removed until the content is less than 300ppm, and tower kettle liquid is discharged;

4) cooling the tower bottom liquid discharged in the step 3) to 85 ℃, feeding the tower bottom liquid into a solid-liquid separation device, separating sodium hydroxide in the tower bottom liquid, overflowing the obtained liquid phase to a dehydration tower, controlling the pressure at the top of the tower to be-90 KPaG, controlling the temperature of the tower bottom to be 125 ℃, removing water until the content is less than 0.15 wt%, and discharging the tower bottom liquid;

5) the tower bottom liquid discharged in the step 4) enters a light component removal tower, the temperature of the tower bottom is controlled to be 135 ℃ under the condition of negative pressure of-92 KPaG, light components are removed, and the tower bottom liquid is discharged;

6) and 5) feeding the tower bottom liquid discharged in the step 5) into a centrifugal machine, adjusting the rotating speed of the centrifugal machine to 7500r/min according to material composition, correspondingly adjusting the deslagging period to 35 min/time, discharging the separated turbid liquid from a liquid outlet, recycling, feeding the discharged clear liquid into a first refining tower, controlling the temperature of the tower bottom to be 135 ℃ under the condition of-96 KPaG, recovering the hexamethylenediamine at the tower top, feeding the discharged tower bottom liquid into a second refining tower, controlling the temperature of the tower bottom to be 142 ℃ under the condition of-98 KPaG, and discharging the tower bottom liquid from a condenser at the tower top of the second refining tower to obtain the target product.

Through detection, the content of the light component organic amine impurity 2-aminocyclopentylmethylamine in the product is 9ppm, the content of the target product 2-hexyltriamine is 95.09%, and the product does not contain sodium hydroxide.

Claims

1. A production system of 2-hexanetriamine is characterized in that: comprises a solid-liquid separation device (9), a dehydration tower (4), a lightness-removing tower (5), a centrifuge (6), a first refining tower (101) and a second refining tower (102),

the material import of solid-liquid separation equipment (9) is used for linking to each other with reactor exhaust's mixture material source through gas-liquid separation, catalyst filtration, dealcoholize, and solid-liquid separation equipment (9) are through overflow pipe (17) to dehydration tower (4) feed, the bottom of the tower bin outlet of dehydration tower (4) is to taking off light tower (5) feed through second pipeline (1b), the bottom of the tower bin outlet of taking off light tower (5) is to centrifuge (6) feed through third pipeline (1c), and the clear liquid export of this centrifuge (6) is to first refined tower (101) feed through fourth pipeline (1d), the bottom of the tower bin outlet of first refined tower (101) is to second refined tower (102) feed through fifth pipeline (1e), the top of the tower bin outlet of second refined tower (102) is connected condenser (19), externally discharges the target product.

2. The system for producing 2-hexanetriamine according to claim 1, wherein: still include reactor (1), filter (2), dealcoholize tower (3), the bottom of reactor (1) sets up the raw materials import, and the top of reactor (1) sets up row material export, through gas-liquid separation device (7), links to each other with the import of filter (2), the export of filter (2) is equipped with dealcoholize charge-in pump (8) through first pipeline (1a) to dealcoholize tower (3) feed on this first pipeline (1a), the bin outlet links to each other with the material import of solid-liquid separation device (9) at the bottom of the tower of dealcoholize tower (3).

3. The system for producing 2-hexanetriamine according to claim 2, wherein: the reactor (1) is provided with a first cooler (11), and the first cooler (11) is a coil or a jacket.

4. The system for producing 2-hexanetriamine according to claim 2, wherein: the gas-liquid separation device (7) comprises a buffer tank (71) and a flash tank (72), the upper portion of the buffer tank (71) is connected with a discharge outlet of the reactor (1), a top outlet of the buffer tank (71) is connected with the flash tank (72) through a compressor and used for providing compressed hydrogen for the reactor (1), a bottom outlet of the buffer tank (71) is connected with the flash tank (72) through a sixth pipeline, a valve is arranged on the sixth pipeline, and a tank bottom outlet of the flash tank (72) is connected with an inlet of the filter (2).

5. The system for producing 2-hexanetriamine according to claim 2, wherein: a filter feeding tank (12) is arranged between the gas-liquid separation device (7) and the filter (2), a second cooler (13) is arranged on the filter feeding tank (12), the second cooler (13) is a coil or a jacket, and a stirrer (14) is arranged in the filter feeding tank (12).

6. The system for producing 2-hexanetriamine according to claim 1, wherein: the solid-liquid separation device (9) comprises a third cooler (15) and a decanter (16), wherein the upstream end of a material medium channel of the third cooler (15) is used for being connected with a mixture source which is discharged from the reactor and is subjected to gas-liquid separation, catalyst filtration and dealcoholization, the downstream end of the material medium channel is connected with an inlet of the decanter (16), and the top of the decanter (16) supplies materials to the dehydration tower (4) through an overflow pipe (17).

7. The system for producing 2-hexanetriamine according to claim 2, wherein: the tower bottom discharge port of the dealcoholization tower (3) is connected with the solid-liquid separation device (9) through a heat medium channel of a heat exchanger (18), and the first pipeline (1a) passes through a cold medium channel of the heat exchanger (18) to supply materials to the dealcoholization tower (3).