CN214528782U - Device for producing hexamethylene diamine by 6-aminocapronitrile hydrogenation - Google Patents
Device for producing hexamethylene diamine by 6-aminocapronitrile hydrogenation Download PDFInfo
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- CN214528782U CN214528782U CN202120797158.1U CN202120797158U CN214528782U CN 214528782 U CN214528782 U CN 214528782U CN 202120797158 U CN202120797158 U CN 202120797158U CN 214528782 U CN214528782 U CN 214528782U
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- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 title claims abstract description 222
- KBMSFJFLSXLIDJ-UHFFFAOYSA-N 6-aminohexanenitrile Chemical compound NCCCCCC#N KBMSFJFLSXLIDJ-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 61
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 51
- 230000018044 dehydration Effects 0.000 claims abstract description 48
- SYECJBOWSGTPLU-UHFFFAOYSA-N hexane-1,1-diamine Chemical compound CCCCCC(N)N SYECJBOWSGTPLU-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000001257 hydrogen Substances 0.000 claims description 59
- 229910052739 hydrogen Inorganic materials 0.000 claims description 59
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 51
- 239000003054 catalyst Substances 0.000 claims description 50
- 238000006243 chemical reaction Methods 0.000 claims description 38
- 239000007788 liquid Substances 0.000 claims description 35
- 239000007787 solid Substances 0.000 claims description 28
- FHKPTEOFUHYQFY-UHFFFAOYSA-N 2-aminohexanenitrile Chemical compound CCCCC(N)C#N FHKPTEOFUHYQFY-UHFFFAOYSA-N 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 239000002699 waste material Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 19
- 239000012295 chemical reaction liquid Substances 0.000 description 11
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 238000004064 recycling Methods 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 238000000926 separation method Methods 0.000 description 5
- 239000007868 Raney catalyst Substances 0.000 description 4
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical group [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 4
- 229910000564 Raney nickel Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229920001778 nylon Polymers 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 230000006641 stabilisation Effects 0.000 description 4
- 238000011105 stabilization Methods 0.000 description 4
- 239000004677 Nylon Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 230000009849 deactivation Effects 0.000 description 2
- 239000007792 gaseous phase Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 229920000305 Nylon 6,10 Polymers 0.000 description 1
- 229920002302 Nylon 6,6 Polymers 0.000 description 1
- BTGRAWJCKBQKAO-UHFFFAOYSA-N adiponitrile Chemical compound N#CCCCCC#N BTGRAWJCKBQKAO-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- YMHQVDAATAEZLO-UHFFFAOYSA-N cyclohexane-1,1-diamine Chemical compound NC1(N)CCCCC1 YMHQVDAATAEZLO-UHFFFAOYSA-N 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model discloses a device of 6-aminocapronitrile hydrogenation production hexane diamine mainly comprises hydrogenation ware, dehydration lightness-removing tower, hexane diamine tower, heavy-duty tower, and the hydrogenation ware is connected with dehydration lightness-removing tower, dehydration lightness-removing tower is connected with hexane diamine tower, hexane diamine tower and heavy-duty tower are connected. The utility model has short production flow, low energy consumption, less by-products and high product quality, and realizes the continuous large-scale production of hexamethylene diamine by continuous hydrogenation of 6-aminocapronitrile.
Description
Technical Field
The utility model belongs to the technical field of organic chemical industry, a technique of hexamethylene diamine is produced by caprolactam is related to, in particular to device of 6-aminocapronitrile hydrogenation production hexamethylene diamine.
Background
Hexamethylenediamine is a key raw material in the nylon industry, is usually used for synthesizing nylon 66 and nylon 610, and then is prepared into products such as nylon resin, nylon fibers, engineering plastics and the like. The industrial production method of the hexamethylene diamine is mainly a adiponitrile catalytic hydrogenation method, and the method produces impurity diaminocyclohexane which has large influence on the quality of nylon products while producing the hexamethylene diamine, and is difficult to separate. At present, with the increasing expansion of caprolactam production capacity and the decreasing price, the caprolactam method is expected to be popularized industrially. The caprolactam method takes caprolactam as a raw material to prepare 6-aminocapronitrile through catalytic ammoniation and dehydration, and the 6-aminocapronitrile is further subjected to catalytic hydrogenation to obtain the hexamethylene diamine.
The existing device for producing hexamethylene diamine by hydrogenating 6-aminocapronitrile is generally an intermittent production process and is not suitable for large-scale continuous production.
Disclosure of Invention
The defect that exists to prior art, the utility model aims to provide a device of 6-aminocapronitrile continuous hydrogenation production hexamethylene diamine, the device have that production flow is short, the energy consumption is low, the accessory substance is few, high product quality's characteristics, realize 6-aminocapronitrile continuous hydrogenation production hexamethylene diamine.
The utility model adopts the technical proposal that: a device for producing hexamethylene diamine by 6-aminocapronitrile hydrogenation mainly comprises a hydrogenation reactor, a dehydration and lightness-removing tower, a hexamethylene diamine tower and a de-heavy tower, wherein the hydrogenation reactor is connected with the dehydration and lightness-removing tower, the dehydration and lightness-removing tower is connected with the hexamethylene diamine tower, and the hexamethylene diamine tower is connected with the de-heavy tower.
The hydrogenation reactor is a fluidized bed reactor, a stirring reactor, a fixed bed reactor or a magnetic stabilization bed reactor.
The fluidized bed reactor is a gas-liquid-solid three-phase fluidized bed hydrogenation reactor and consists of two or more similar reaction pipes, a gas-liquid separator and a liquid-solid separator, wherein the reaction pipes ascend to the gas-liquid separator, and the lower part of the gas-liquid separator is connected with the liquid-solid separator; the gas-liquid separator gas-phase outlet is connected with a hydrogen circulating compressor; the liquid-solid separator is provided with a waste catalyst discharge port; the reaction tube bottom connect material inlet pipe and hydrogen inlet pipe, reaction material and the hydrogen that comes from hydrogen booster compressor and hydrogen circulating compressor are from the material inlet pipe and the hydrogen inlet pipe feeding of reaction tube bottom respectively.
The gas-liquid separator gas-phase outlet is connected with the hydrogen washing tower, the hydrogen washing tower is provided with a circulating cooler, the inlet of the circulating cooler is connected with the outlet at the lower part of the hydrogen washing tower, and the outlet of the circulating cooler is connected with the upper part of the hydrogen washing tower.
The stirring reactor is a horizontal stirring reactor or a vertical stirring reactor.
The stirring reactor or the magnetic stabilization bed reactor is connected with a gas-liquid-solid three-phase separator.
And a gas-liquid separator is connected behind the fixed bed reactor.
And a filter is arranged between the hydrogenation reactor and the dehydration and lightness-removing tower, and solid matters such as a catalyst and the like carried by hydrogenation reaction liquid are filtered.
The gas phase outlet at the top of the dehydration and lightness-removing tower is connected with a condenser and a reflux tank, water and light components are separated from the top of the tower, and the bottom of the dehydration and lightness-removing tower is connected with a hexamethylenediamine tower.
The gas phase outlet at the top of the hexamethylenediamine tower is connected with a condenser and a reflux tank, hexamethylenediamine is separated from the top of the tower, and the bottom of the tower is connected with a de-weighting tower; or the gas phase outlet at the top of the hexamethylenediamine tower is connected with a dehydration and lightness removal tower, a hexamethylenediamine side draw outlet is arranged at the higher section of the tower, a condenser is connected in parallel, and the tower bottom is connected with a de-heavy tower.
An aminocapronitrile tower is arranged behind the hexamethylenediamine tower, the bottom of the hexamethylenediamine tower is connected with the aminocapronitrile tower, 6-aminocapronitrile is extracted from the top of the hexamethylenediamine tower, and the bottom of the hexamethylenediamine tower is connected with a de-heavy tower.
And a heavy component outlet is arranged at the bottom of the de-heavy tower, and the gas phase at the top of the de-heavy tower is sent to a hexamethylenediamine tower after passing through a condenser.
The dehydration and lightness-removing tower, the hexamethylenediamine tower, the aminocapronitrile tower and the de-heavy tower are connected with a vacuum system.
The utility model discloses in, through connecting such as pipeline, valve, flange between each equipment, can establish relevant affiliated facilities such as pump, jar.
The production process for producing hexamethylene diamine by using the device for producing hexamethylene diamine by hydrogenating 6-aminocapronitrile comprises the following steps:
mixing a catalyst, 6-aminocapronitrile and a cocatalyst in a hydrogenation reaction feeding tank, then feeding the mixture into a hydrogenation reactor, feeding fresh hydrogen and circulating hydrogen into the hydrogenation reactor together, and reacting at the temperature of 30-120 ℃ and the pressure of 0-12 MPaG.
Wherein the catalyst is Raney nickel, Raney cobalt or Raney nickel cobalt;
wherein the cocatalyst is NaOH, KOH, CH3CH2ONa、CH3Any one or a combination of at least two of ONa;
wherein the mass ratio of the catalyst to the 6-aminocapronitrile is 0.05-0.5: 1, the mass ratio of the cocatalyst to the 6-aminocapronitrile is 0.001-0.1: 1, and the molar ratio of the hydrogen to the 6-aminocapronitrile is 2-100: 1.
When a fluidized bed reactor is adopted, unreacted hydrogen and liquid in the gas-liquid separator are separated, and the hydrogen is pressurized and recycled by a hydrogen circulating compressor. The lower part of the gas-liquid separator is provided with a liquid-solid separator, and the bottom tip part of the liquid-solid separator is provided with a waste catalyst discharge outlet. In order to maintain the concentration and activity of the catalyst in the reactor, a certain amount of catalyst is discharged from the catalyst circulation system to a catalyst washing tank, the catalyst is washed with water in the tank, the washed catalyst is discharged from the bottom, a part of the catalyst is returned to a catalyst feeder for recycling, and a part of the catalyst is discharged after passivation treatment.
When a stirring reactor or a magnetic stabilization bed reactor is adopted, the 6-aminocapronitrile reacts with hydrogen, then the reaction material is sent to a gas-liquid-solid separator for separation, the separated catalyst is returned to a hydrogenation reactor, the hydrogen is recycled after being treated and compressed, and the reaction liquid is sent to a dehydration and lightness-removing tower.
When a fixed bed reactor is adopted, 6-aminocapronitrile reacts with hydrogen, the reaction material is sent to a gas-liquid separator for separation, the hydrogen is recycled after being treated and compressed, and the reaction liquid is sent to a dehydration and lightness-removing tower.
And (3) sending the crude hexamethylenediamine to a dehydration and lightness removal tower, wherein the temperature at the top of the dehydration and lightness removal tower is 20-50 ℃, the pressure at the top of the dehydration and lightness removal tower is 15-95 mmHgA (absolute pressure), the water at the top of the dehydration and lightness removal tower and HMI are sent to a wastewater pretreatment system after being condensed, and the crude hexamethylenediamine at the bottom of the dehydration and lightness removal tower is sent to a hexamethylenediamine tower.
The temperature of the top of the hexamethylenediamine tower is 85-105 ℃, the pressure of the top of the hexamethylenediamine tower is 15-35 mmHgA, and refined hexamethylenediamine is extracted from the top of the hexamethylenediamine tower and is sent to a hexamethylenediamine storage tank in a tank field. The tower bottom recombination is sent to a de-heavy tower or an aminocapronitrile tower.
The temperature of the top of the de-heavy tower is 85-135 ℃, the pressure of the top of the de-heavy tower is 15-100 mmHgA, the components at the top of the de-heavy tower return to the hexamethylenediamine tower to recover hexamethylenediamine products, and the heavy components are extracted at the bottom of the de-heavy tower.
And an aminocapronitrile tower can also be arranged, heavy components at the bottom of the hexamethylenediamine tower are sent to the aminocapronitrile tower, the temperature at the top of the aminocapronitrile tower is 115-135 ℃, the pressure at the top of the aminocapronitrile tower is 15-35 mmHgA, 6-aminocapronitrile is extracted from the top of the tower and used as a raw material to return to the hydrogenation reactor, and materials at the bottom of the tower are sent to the de-heavy tower.
The utility model discloses an effect:
the utility model discloses device of 6-aminocapronitrile hydrogenation production hexamethylene diamine, its production procedure is short, the energy consumption is low, the accessory substance is few, product quality is high, has realized the scale continuous production of 6-aminocapronitrile continuous hydrogenation production hexamethylene diamine.
Drawings
FIG. 1 is a schematic diagram of a 6-aminocapronitrile hydrogenation apparatus of the present invention for producing hexamethylenediamine;
FIG. 1-hydrogenation feed tank; 2-a hydrogenation reactor; 3-hydrogen recycle compressor; 5-a filter; 6-dehydration lightness-removing tower; a 7-hexanediamine column; 8-a de-weighting tower; 9-a vacuum system; 10-hydrogen booster compressor; 11-gas-liquid-solid separator.
FIG. 2 is a schematic diagram of a device for producing hexamethylenediamine by fluidized bed hydrogenation of 6-aminocapronitrile;
FIG. 1-hydrogenation feed tank; 2-1-a fluidized bed reactor; 3-hydrogen recycle compressor; 5-a filter; 6-dehydration lightness-removing tower; a 7-hexanediamine column; 8-a de-weighting tower; 9-a vacuum system; 10-hydrogen pressure boosting compressor.
FIG. 3 is a schematic diagram of the apparatus for producing hexamethylenediamine by fixed bed hydrogenation of 6-aminocapronitrile according to the present invention;
FIG. 1-hydrogenation feed tank; 2-2-fixed bed reactor; 3-hydrogen recycle compressor; 4-a gas-liquid separator; 5-a filter; 6-dehydration lightness-removing tower; a 7-hexanediamine column; 8-a de-weighting tower; 9-a vacuum system; 10-hydrogen pressure boosting compressor.
Detailed Description
The following examples further illustrate the present invention, but the present invention is not limited to these examples.
As can be seen from figure 1, the utility model relates to a device for producing hexamethylene diamine by 6-aminocapronitrile hydrogenation, which mainly comprises a hydrogenation reactor 2, a dehydration lightness-removing tower 6, a hexamethylene diamine tower 7 and a de-heavy tower 8, wherein the bottom of the hydrogenation reactor is connected with a material feeding pipe and a hydrogen feeding pipe. The back of the hydrogenation reactor 2 is connected with a gas, liquid and solid three-phase separator 11, a gas phase outlet is connected with a hydrogen circulating compressor, a solid phase outlet is a catalyst outlet and returns to the hydrogenation reaction feeding tank 1, a liquid phase outlet is connected with a dehydration and lightness-removing tower 6 through a filter 5, a gas phase outlet at the top of the dehydration and lightness-removing tower 6 is connected with a condenser, and the bottom of the dehydration and lightness-removing tower is connected with a hexamethylenediamine tower 7; the bottom of the heavy component removing tower is provided with a heavy component outlet, and a gas phase outlet at the top of the tower is connected with the hexamethylenediamine tower. The dehydration and lightness removal tower, the hexamethylenediamine tower and the de-heavy tower are all connected with a vacuum system.
The utility model discloses can also add between the hexanediamine tower and the heavy tower of taking off and establish aminocapronitrile tower, the hexanediamine tower bottom links to each other with aminocapronitrile tower, and 6-aminocapronitrile is extracted at the top of the tower, and the tower bottom links to each other with the heavy tower of taking off.
As can be seen from figure 2, the utility model relates to a device for producing hexamethylene diamine by 6-aminocapronitrile hydrogenation, which mainly comprises a fluidized bed hydrogenation reactor 2-1, a dehydration lightness-removing tower 6, a hexamethylene diamine tower 7 and a de-weighting tower 8, wherein the fluidized bed hydrogenation reactor is a gas, liquid and solid three-phase fluidized bed hydrogenation reactor and consists of two or more similar reaction tubes, a gas-liquid separator and a liquid-solid separator, the bottom of each reaction tube is connected with a material feeding tube and a hydrogen feeding tube, the reaction tubes ascend to the gas-liquid separator, and the lower part of the gas-liquid separator is connected with the liquid-solid separator; the gas-liquid separator gas-phase outlet is connected with a hydrogen circulating compressor; a solid phase outlet of the liquid-solid separator is a catalyst outlet and returns to the hydrogenation reaction feeding tank 1, a liquid phase outlet is connected with a dehydration and lightness-removing tower 6 through a filter 5, a gas phase outlet at the top of the dehydration and lightness-removing tower 6 is connected with a condenser, and the bottom of the dehydration and lightness-removing tower is connected with a hexamethylenediamine tower 7; the bottom of the heavy component removing tower is provided with a heavy component outlet, and a gas phase outlet at the top of the tower is connected with the hexamethylenediamine tower. The dehydration and lightness removal tower, the hexamethylenediamine tower and the de-heavy tower are all connected with a vacuum system.
The utility model discloses can also add between the hexanediamine tower and the heavy tower of taking off and establish aminocapronitrile tower, the hexanediamine tower bottom links to each other with aminocapronitrile tower, and 6-aminocapronitrile is extracted at the top of the tower, and the tower bottom links to each other with the heavy tower of taking off.
As can be seen from figure 3, the utility model relates to a 6-aminocapronitrile hydrogenation produces device of hexanediamine, mainly by fluidized bed hydrogenation ware 2-2, dehydration lightness-removing tower 6, hexanediamine tower 7, heavy-duty tower 8 constitutes, the solid phase export of fixed bed hydrogenation ware 2-2 is the catalyst export, return hydrogenation feed tank 1, upper portion export meets vapour and liquid separator 4, the gaseous phase export is connected with hydrogen cycle compressor, the liquid phase export passes through filter 5 and is connected with dehydration lightness-removing tower 6, the gaseous phase export in dehydration lightness-removing tower 6 top of the tower is connected with the condenser, dehydration lightness-removing tower bottom is connected with hexanediamine tower 7; the bottom of the heavy component removing tower is provided with a heavy component outlet, and a gas phase outlet at the top of the tower is connected with the hexamethylenediamine tower. The dehydration and lightness removal tower, the hexamethylenediamine tower and the de-heavy tower are all connected with a vacuum system.
The utility model discloses can also add between the hexanediamine tower and the heavy tower of taking off and establish aminocapronitrile tower, the hexanediamine tower bottom links to each other with aminocapronitrile tower, and 6-aminocapronitrile is extracted at the top of the tower, and the tower bottom links to each other with the heavy tower of taking off.
The production process of hexamethylenediamine by hydrogenation of 6-aminocapronitrile is described below with reference to the specific examples and the drawings.
Example 1:
this example used the apparatus of FIG. 2 to produce hexamethylenediamine.
The catalyst, the 6-aminocapronitrile and the cocatalyst are mixed in a hydrogenation reaction feeding tank and then are sent to a gas-liquid-solid three-phase fluidized bed reactor, the reactor is provided with three reaction tubes, reaction materials and hydrogen from a hydrogen boosting compressor and a hydrogen circulating compressor are supplied from the bottom of the reaction tubes respectively, the reaction is carried out at the temperature of 60-90 ℃ and under the pressure of 2.0-2.5 MPaG, the hydrogen and the reaction liquid rise together from the reaction tubes to reach a gas-liquid separator, and the reaction is basically finished. The reaction is exothermic and the heat of reaction is removed by external cooling water.
Wherein the catalyst is Raney nickel, the cocatalyst is NaOH, and the mass ratio of the catalyst to 6-aminocapronitrile is 0.05-0.3: 1, the mass ratio of the cocatalyst to the 6-aminocapronitrile is 0.001-0.1: 1, and the molar ratio of the hydrogen to the 6-aminocapronitrile is 2-100: 1.
And separating unreacted hydrogen from liquid in the gas-liquid separator, and pressurizing and recycling the hydrogen by a hydrogen recycling compressor. The lower part of the gas-liquid separator is provided with a liquid-solid separator, and the top tip part of the liquid-solid separator is provided with a waste catalyst discharge outlet. In order to maintain the concentration and activity of the catalyst in the reactor, certain amount of catalyst is discharged from the catalyst circulating system to a discharged catalyst washing tank, the catalyst is washed with water in the tank, the washed catalyst is discharged from the bottom, part of the catalyst is returned to the catalyst feeder for recycling, and part of the catalyst is discharged to a catalyst deactivator for deactivation and then discharged.
And pumping the crude hexamethylenediamine into a dehydration and lightness-removing tower, separating water, HMI (human machine interface) and the crude hexamethylenediamine solution at the temperature of 20-50 ℃ at the top of the tower and under the pressure of 15-95 mmHgA at the top of the tower, pumping the water, HMI and the crude hexamethylenediamine solution from the top of the tower, conveying the separated water to a wastewater pretreatment system, and conveying the crude hexamethylenediamine solution at the bottom of the tower to a hexamethylenediamine tower for treatment.
And (3) under the conditions that the temperature of the top of the hexamethylenediamine tower is 85-105 ℃ and the pressure of the top of the hexamethylenediamine tower is 15-35 mmHgA, delivering heavy components from the bottom of the tower to a de-heavy tower. And (4) collecting refined hexamethylene diamine at the top of the tower, and sending the refined hexamethylene diamine to a hexamethylene diamine storage tank in a tank field.
And (3) a heavy component removing tower, wherein the tower top components are returned to the hexamethylenediamine tower to recover the hexamethylenediamine product, and heavy components are extracted from the tower bottom under the conditions that the tower top temperature is 85-135 ℃ and the tower top pressure is 15-100 mmHgA.
And an aminocapronitrile tower can be arranged behind the hexamethylenediamine tower, heavy components at the bottom of the hexamethylenediamine tower are fed into the aminocapronitrile tower, 6-aminocapronitrile is extracted from the top of the tower under the conditions that the temperature at the top of the tower is 115-135 ℃ and the pressure at the top of the tower is 15-35 mmHgA, the 6-aminocapronitrile is used as a raw material and returned to the hydrogenation reactor, and the material discharged from the bottom of the tower is fed to the tar stripping tower.
The conversion rate of 6-aminocapronitrile is 99-100%, the purity of hexamethylene diamine reaches 99.95% (mass percentage), and the yield of hexamethylene diamine reaches 96-97%.
Example 2
This example used the apparatus of FIG. 1 to produce hexamethylenediamine. The hydrogenation reactor is a horizontal stirring reactor or a vertical continuous stirring reactor.
6-aminocapronitrile and hydrogen enter a reactor to react at the temperature of 90-110 ℃ and the pressure of 4.0-11.0 MPa, reaction liquid is sent to a gas-liquid-solid separator for separation after the reaction, the separated catalyst is returned to a hydrogenation reactor, the hydrogen is recycled after being treated and compressed, and the reaction liquid is sent to a dehydration and lightness-removing tower.
The conversion rate of 6-aminocapronitrile is 99-100%, the purity of hexamethylene diamine reaches 99.95% (mass percentage), and the yield of hexamethylene diamine reaches 96-97%.
Example 3
This example used the apparatus of FIG. 1 to produce hexamethylenediamine. The hydrogenation reactor is a magnetic stabilization bed reactor.
6-aminocapronitrile and hydrogen enter a reactor to react at the temperature of 90-110 ℃ and the pressure of 4.0-11.0 MPa, reaction liquid is sent to a gas-liquid-solid separator for separation after the reaction, the separated catalyst is returned to a hydrogenation reactor, the hydrogen is recycled after being treated and compressed, and the reaction liquid is sent to a dehydration and lightness-removing tower.
The conversion rate of 6-aminocapronitrile is 99-100%, the purity of hexamethylene diamine reaches 99.95% (mass percentage), and the yield of hexamethylene diamine reaches 96-97%.
Example 4
This example used the apparatus of FIG. 3 to produce hexamethylenediamine. The hydrogenation reactor is a fixed bed reactor.
6-aminocapronitrile and hydrogen enter a reactor to react at the temperature of 90-110 ℃ and the pressure of 4.0-11.0 MPa, reaction liquid is sent to a gas-liquid separator for separation after the reaction, the hydrogen is recycled after being treated and compressed, and the reaction liquid is sent to a dehydration and lightness-removing tower.
The conversion rate of 6-aminocapronitrile is 98-99%, the purity of hexamethylene diamine reaches 99.95% (mass percentage), and the yield of hexamethylene diamine reaches 96-97%.
Example 5
This example used the apparatus of FIG. 2 to produce hexamethylenediamine.
The catalyst, the 6-aminocapronitrile and the cocatalyst are mixed in a hydrogenation reaction feeding tank and then are sent to a gas-liquid-solid three-phase fluidized bed reactor, the reactor is provided with three reaction tubes, reaction materials and hydrogen from a hydrogen boosting compressor and a hydrogen circulating compressor are supplied from the bottom of the reaction tubes respectively, the reaction is carried out at the temperature of 60-90 ℃ and under the pressure of 2.0-2.5 MPaG, the hydrogen and the reaction liquid rise together from the reaction tubes to reach a gas-liquid separator, and the reaction is basically finished. The reaction is exothermic and the heat of reaction is removed by external cooling water.
Wherein the catalyst is Raney nickel, the cocatalyst is NaOH, and the mass ratio of the catalyst to 6-aminocapronitrile is 0.05-0.3: 1, the mass ratio of the cocatalyst to the 6-aminocapronitrile is 0.001-0.1: 1, and the molar ratio of the hydrogen to the 6-aminocapronitrile is 2-100: 1.
And separating unreacted hydrogen from liquid in the gas-liquid separator, and pressurizing and recycling the hydrogen by a hydrogen recycling compressor. The lower part of the gas-liquid separator is provided with a liquid-solid separator, and the top tip part of the liquid-solid separator is provided with a waste catalyst discharge outlet. In order to maintain the concentration and activity of the catalyst in the reactor, certain amount of catalyst is discharged from the catalyst circulating system to a discharged catalyst washing tank, the catalyst is washed with water in the tank, the washed catalyst is discharged from the bottom, part of the catalyst is returned to the catalyst feeder for recycling, and part of the catalyst is discharged to a catalyst deactivator for deactivation and then discharged.
And pumping the crude hexamethylenediamine into a dehydration and lightness-removing tower, separating water, HMI (human machine interface) and the crude hexamethylenediamine solution at the temperature of 20-50 ℃ at the top of the tower and under the pressure of 15-95 mmHgA at the top of the tower, pumping the water, HMI and the crude hexamethylenediamine solution from the top of the tower, conveying the separated water to a wastewater pretreatment system, and conveying the crude hexamethylenediamine solution at the bottom of the tower to a hexamethylenediamine tower for treatment.
And (3) under the conditions that the temperature of the top of the hexamethylenediamine tower is 85-105 ℃ and the pressure of the top of the hexamethylenediamine tower is 15-35 mmHgA, delivering heavy components from the bottom of the tower to a de-heavy tower. And (4) collecting refined hexamethylene diamine at the top of the tower, and sending the refined hexamethylene diamine to a hexamethylene diamine storage tank in a tank field.
Feeding the heavy components at the bottom of the hexamethylenediamine tower into an aminocapronitrile tower, wherein the tower top temperature of the aminocapronitrile tower is 115-135 ℃, the tower top pressure is 15-35 mmHgA, 6-aminocapronitrile is extracted from the tower top and used as a raw material to return to a hydrogenation reactor, and the material at the bottom of the tower is fed into a de-heavy tower.
And (3) a heavy component removing tower, wherein the tower top components are returned to the hexamethylenediamine tower to recover the hexamethylenediamine product, and heavy components are extracted from the tower bottom under the conditions that the tower top temperature is 85-135 ℃ and the tower top pressure is 15-100 mmHgA.
And an aminocapronitrile tower can be arranged behind the hexamethylenediamine tower, heavy components at the bottom of the hexamethylenediamine tower are fed into the aminocapronitrile tower, 6-aminocapronitrile is extracted from the top of the tower under the conditions that the temperature at the top of the tower is 115-135 ℃ and the pressure at the top of the tower is 15-35 mmHgA, the 6-aminocapronitrile is used as a raw material and returned to the hydrogenation reactor, and the material discharged from the bottom of the tower is fed to the tar stripping tower.
The conversion rate of the 6-aminocapronitrile is about 100 percent, the purity of the hexamethylene diamine reaches 99.95 percent (mass percentage), and the yield of the hexamethylene diamine reaches 97-98 percent.
Claims (10)
1. The device for producing the hexamethylene diamine by hydrogenating the 6-aminocapronitrile mainly comprises a hydrogenation reactor, a dehydration and lightness-removing tower, a hexamethylene diamine tower and a de-heavy tower, and is characterized in that: the hydrogenation reactor is connected with a dehydration and lightness removal tower, the dehydration and lightness removal tower is connected with a hexamethylenediamine tower, and the hexamethylenediamine tower is connected with a de-heavy tower.
2. The apparatus for producing hexamethylenediamine by hydrogenating 6-aminocapronitrile according to claim 1, wherein the hydrogenation reactor is a fluidized bed reactor, a stirred reactor, a fixed bed reactor or a magnetically stabilized bed reactor; the stirring reaction is a horizontal stirring reactor or a vertical stirring reactor.
3. The apparatus for producing hexanediamine by hydrogenating 6-aminocapronitrile according to claim 1, wherein a filter is disposed between the hydrogenation reactor and the dehydration and lightness-removing column.
4. The apparatus for producing hexanediamine by hydrogenating 6-aminocapronitrile according to claim 1, wherein the gas phase outlet at the top of the dehydration and lightness-removing column is connected with a condenser, water and light components are separated from the top of the dehydration and lightness-removing column, and the bottom of the dehydration and lightness-removing column is connected with the hexanediamine column; or
The gas phase outlet at the top of the hexamethylenediamine tower is connected with a condenser, hexamethylenediamine is separated from the top of the tower, and the bottom of the tower is connected with a de-heavy tower; or
The gas phase outlet at the top of the hexamethylenediamine tower is connected with a dehydration and lightness removal tower, a hexamethylenediamine side draw outlet is arranged at the higher section of the tower, and the tower bottom is connected with a weight removal tower.
5. The apparatus for producing hexanediamine by 6-aminocapronitrile hydrogenation according to claim 1, wherein the hexanediamine column is followed by an aminocapronitrile column, the bottom of the hexanediamine column is connected with the aminocapronitrile column, 6-aminocapronitrile is extracted from the top of the hexanediamine column, and the bottom of the hexanediamine column is connected with the de-heavy column.
6. The apparatus for producing hexanediamine by hydrogenating 6-aminocapronitrile according to claim 1, wherein the dehydration and lightness-removing column, the hexanediamine column and the de-heaving column are connected with a vacuum system.
7. The apparatus for producing hexanediamine by hydrogenating 6-aminocapronitrile according to claim 1, wherein the heavy component removing column is provided with a heavy component outlet at the bottom and a gas phase outlet at the top is connected with the hexanediamine column.
8. The apparatus for producing hexanediamine by 6-aminocapronitrile hydrogenation according to claim 2, wherein the fluidized bed reactor is a gas, liquid and solid three-phase fluidized bed reactor, and comprises two or more similar reaction tubes, a gas-liquid separator and a liquid-solid separator, wherein the reaction tubes are lifted to the gas-liquid separator, and the lower part of the gas-liquid separator is connected with the liquid-solid separator; the gas-liquid separator gas-phase outlet is connected with a hydrogen circulating compressor; the liquid-solid separator is provided with a waste catalyst discharge port; the bottom of the reaction tube is connected with a material feeding tube and a hydrogen feeding tube.
9. The apparatus according to claim 8, wherein the gas-liquid separator has a gas outlet connected to a hydrogen scrubber, the hydrogen scrubber is provided with a recycle cooler, an inlet of the recycle cooler is connected to a lower outlet of the hydrogen scrubber, and an outlet of the recycle cooler is connected to an upper part of the hydrogen scrubber.
10. The apparatus for producing hexanediamine by hydrogenating 6-aminocapronitrile according to claim 2, wherein a gas, liquid and solid three-phase separator is connected after the stirred reactor or the magnetically stabilized bed reactor; the fixed bed reactor is connected with a gas-liquid separator.
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