CN109776333A - The technique and reaction unit of 2,5- dichloronitrobenzene uninanned platform 2,5- dichloroaniline - Google Patents
The technique and reaction unit of 2,5- dichloronitrobenzene uninanned platform 2,5- dichloroaniline Download PDFInfo
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- CN109776333A CN109776333A CN201910177093.8A CN201910177093A CN109776333A CN 109776333 A CN109776333 A CN 109776333A CN 201910177093 A CN201910177093 A CN 201910177093A CN 109776333 A CN109776333 A CN 109776333A
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- dichloronitrobenzene
- dichloroaniline
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Abstract
The present invention relates to 2,5- dichloronitrobenzene uninanned platform 2, the technique of 5- dichloroaniline, using fixed bed continuous reacting device, by pure raw material 2,5- dichloronitrobenzene is passed into the fixed bed reactors equipped with catalyst in the molten state together with reductive hydrogen, obtains product 2,5- dichloroaniline and a small amount of water；The limitation that Hydrogen Vapor Pressure in reaction temperature, reaction front and back and reaction has comparison stringent, and hydrogen is recycled.Technique of the invention is environmentally protective, and reactor product is without dividing water directly for subsequent use, and no dechlorinated side product, product purity is not less than 99.9%；Not only the security risk of hydrogenation reaction had been reduced, but also has improved the production efficiency of device.
Description
Technical field
The invention belongs to a kind of synthetic technologys of 2,5- dichloroaniline.
Background technique
Although the production technology of synthesis 2,5- dichloroaniline has industrialized, in actual production, still remain raw
Produce that cost is excessively high, the problems such as product quality and yield are unstable, seriously polluted, and substantially intermittently to change based on hydrogenation technique.Cause
This, a kind of efficient stable of research and development, environmental-friendly, cheap 2,5- dichloroaniline be continuously synthesizing to technique and
Reaction unit, to the security risk, the automatic controlling level for improving device, raising device production efficiency etc. for reducing hydrogenation reaction
Have great importance.
The applicant's enterprise staff be published in December, 2018 " being printed when chemical industry " paper " fixed bed continuously hydrogen adding synthesis 2,
The technical study of 5- dichloroaniline " describes the continuous production technology of 2, the 5- dichloroaniline synthesis of solvent dissolution, provides
The suitable parameters such as catalyst and temperature, pressure, but the amount due to that cannot control hydrogen, there are side reactions, and the purity of finished product is not
Enough high, reaction speed is not fast enough in solution.
Main reaction equation:
；
Side reaction equation:
。
Summary of the invention
Goal of the invention: a kind of solvent-free 2,5- dichloronitrobenzene synthesis 2,5- bis- substantially without side reaction, no three wastes is provided
The technique and reaction unit of chloroaniline.
Technical solution:
The synthesis technology of 2,5- dichloroaniline of the invention, comprising the following steps:
Step 1: filling required catalyst in the reactor, it is passed through excessive reducibility gas hydrogen, adjusts the temperature of reactor
Degree is 80 DEG C ~ 140 DEG C, pressure P is 1.0MPa ~ 1.5MPa, is then passed through by the way of serialization charging into reactor molten
2, the 5- dichloronitrobenzene melted, carries out hydrogenation reaction, and obtained material is 2,5- dichloroaniline and a small amount of water；Without dividing water direct
It is used for subsequent synthesis, no three wastes generates.
Step 2: unreacted hydrogen is recycled, by drying and dehydrating, reuse is into step 1.
In the present invention, due to solvent-free doping and volatilization, reaction temperature described in step 1 is preferably 125-140 DEG C,
To accelerate reaction speed；By increase reaction pressure, the density of hydrogen is improved, it is abundant with 2, the 5- dichloronitrobenzene of pure molten
Haptoreaction, the reaction pressure P is preferably 1.3-1.5MPa, so that reaction accelerates, feed stock conversion is high, and reaction is abundant.
In the present invention, the volume space velocity of melting 2, the 5- dichloronitrobenzene is greatly improved than documents.It can achieve
0.69h-1-1.01h-1。
Hydrogen Vapor Pressure P1 before reactor, the Hydrogen Vapor Pressure P2 after reactor, by control air inlet, reactor
Pressure, outlet guarantee P1-P2=3/8P-5/8P, while main reaction is sufficiently completed, accurately control hydrogen addition
The molar ratio of the dosage of reaction, two kinds of raw materials is appropriate, almost without the generation of side reaction, so that the purity of finished product obtains greatly
Guarantee, reach 99.9% or so.After optimizing adjustment to pressure, fixed bed processing capacity can be improved 3 times or more, not
The reducibility gas of reaction is reusable, save the cost and environmental-friendly, reduces the security risk of hydrogenation reaction, improves device
Automatic controlling level and production efficiency.
Referring to documents, the catalyst that can be used is catalyzed the present invention for Pd/C, Pt/C, Ru/C or Rh/C of 3-5%
Agent.
In a molten state due to not having solvent in raw material, catalyst can come into full contact with raw material, improve catalysis effect
The dosage of rate, catalyst can be less.Catalyst used is preferably Ru/C the Rh/C catalyst of 3-4%.
In above-mentioned technique, used reaction unit has and flows through sequentially connected hydrogen supply on pipeline in hydrogen
Device, filter, flow and pressure-regulating valve A, fixed bed reactors (containing pressure gauge), flow and pressure-regulating valve B, product storage
Batch can, tail gas tank, drier, connection hydrogen gas supplying apparatus after drier.
Separately successively there is 2,5- dichloronitrobenzene feeding mechanism, metering device and one-way cock, be connected to fixed bed reaction
Device.
Or separately there is controller, it is separately connected control flow and pressure-regulating valve A, pressure gauge, flow and pressure is adjusted
Valve B collects the pressure of three kinds of pressure signals and three position hydrogen of auto-control, so that reducing manual control, further increases
The safety and reliability of reaction efficiency and reaction.
The present invention has the advantage that compared with prior art
1. 2,5- dichloronitrobenzene is fixed under the conditions of the present invention can be 80 DEG C ~ 140 DEG C in temperature, pressure is 1.0MPa ~ 1.5MPa
Bed serialization hydrogenation synthesis 2,5- dichloroaniline, raw material 2, the conversion ratio of 5- dichloronitrobenzene reach 100%, no dechlorinated side product,
2,5- dichloroaniline gas phase quality purity is not less than 99.9%.
2. the material that catalytic hydrogenation of the present invention obtains be 2,5- dichloroaniline and a small amount of water, it is subsequent without dividing water directly to supply
Synthesis uses, and no three wastes generates；And unreacted reducibility gas is can be recycled, save the cost and environmental-friendly.
3. raw material of the present invention is melting 2,5- dichloronitrobenzene, this technique is not necessarily to other solvents or reagent, technique letter
It is single, it economizes on resources, green and low cost.
4. it is simple and easily operated using fixed bed device, the peace of hydrogenation reaction can be reduced using fixed-bed reactor
Full blast danger, the automatic controlling level and production efficiency for improving device.
Detailed description of the invention
Fig. 1 is a kind of reaction unit structural schematic diagram of the invention；
In figure, 1- hydrogen gas supplying apparatus, 2- filter, 3- flow and pressure-regulating valve A, 4- fixed bed reactors, 5- flow and
Pressure-regulating valve B, 6- product storage tank, 7- tail gas tank, 8- drier, 9--2,5- dichloronitrobenzene feeding mechanism, 10- metering
Device, 11- one-way cock.
Specific embodiment
Below by embodiment, technical solution of the present invention is described in further detail.
Embodiment 1
Step 1: filling required catalyst in fixed bed reactors, it is passed through reducibility gas, adjusts fixed bed reactors
Then temperature and pressure are passed through the 2,5- of raw material melting with metering pump by the way of serialization charging into fixed bed reactors
Dichloronitrobenzene carries out hydrogenation reaction under required temperature and pressure condition；The melting 2,5- dichloronitrobenzene and 2,5- bis-
The volume space velocity of chlorobenzene amine blends is 0.52-0.69h-1, the reaction temperature is 80 DEG C ~ 90 DEG C, and the reaction pressure is
1.22MPa。
Step 2: the material that catalytic hydrogenation obtains in step 1 is 2,5- dichloroaniline and a small amount of water, without dividing water direct
It is used for subsequent synthesis, no three wastes generates, and unreacted reducibility gas is Ke Xunhuanliyong in step 1.
Table 1 is the catalytic hydrogenation result of embodiment 1:
1 solventless method of table tentatively probes into activity rating data
Embodiment 2
Step 1: filling required catalyst in fixed bed reactors, it is passed through reducibility gas, adjusts fixed bed reactors
Then temperature and pressure are passed through the 2,5- of raw material melting with metering pump by the way of serialization charging into fixed bed reactors
Dichloronitrobenzene carries out hydrogenation reaction under required temperature and pressure condition；The melting 2,5- dichloronitrobenzene and 2,5- bis-
The volume space velocity of chlorobenzene amine blends is 0.78h-1~1.01h-1, the reaction temperature is 90 DEG C ~ 105 DEG C, the reaction pressure
For 1.24MPa.
Step 2: the material that catalytic hydrogenation obtains in step 1 is 2,5- dichloroaniline and a small amount of water, without dividing water direct
It is used for subsequent synthesis, no three wastes generates, and unreacted reducibility gas is Ke Xunhuanliyong in step 1.
Table 2 is the catalytic hydrogenation result of embodiment 2:
The secondary verifying activity rating data of 2 solventless method of table
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, all technologies according to the present invention
Essence any simple modification to the above embodiments, change and equivalent structural changes, still fall within the technology of the present invention side
In the protection scope of case.
Claims (7)
1.2,5- dichloronitrobenzene uninanned platforms 2, the technique of 5- dichloroaniline, it is characterised in that: the following steps are included:
Step 1: filling required catalyst in the reactor, it is passed through excessive reducibility gas hydrogen, adjusts the temperature of reactor
Degree is 80 DEG C ~ 140 DEG C, pressure P is 1.0MPa ~ 1.5MPa, is then passed through by the way of serialization charging into reactor molten
2, the 5- dichloronitrobenzene melted, carries out hydrogenation reaction, and obtained material is 2,5- dichloroaniline and a small amount of water；
Step 2: unreacted hydrogen is recycled, by drying and dehydrating, reuse to step one kind.
2. 2,5- dichloronitrobenzene uninanned platform 2 described in accordance with the claim 1, the technique of 5- dichloroaniline, feature exists
In: reaction temperature described in step 1 is 125-140 DEG C, and the reaction pressure P is 1.3-1.5MPa.
3. 2,5- dichloronitrobenzene uninanned platform 2 described in accordance with the claim 1, the technique of 5- dichloroaniline, feature exists
In: the volume space velocity of the melting 2,5- dichloronitrobenzene is 0.69h-1-1.01h-1；Hydrogen Vapor Pressure P1 before reactor, instead
Answer Hydrogen Vapor Pressure P2, P1-P2=3/8P ~ 5/8P after device.
4. 2,5- dichloronitrobenzene uninanned platform 2 described in accordance with the claim 1, the technique of 5- dichloroaniline, feature exists
In: catalyst used is Pd/C, Pt/C, Ru/C or Rh/C catalyst of 3-5%.
5. 2,5- dichloronitrobenzene uninanned platform 2 according to claim 4, the technique of 5- dichloroaniline, feature exist
In: catalyst used is Ru/C the Rh/C catalyst of 3-4%.
6. one kind 2,5- dichloronitrobenzene uninanned platform 2, the device of 5- dichloroaniline, it is characterised in that: use claim
Any one technique in 1-5 successively has hydrogen gas supplying apparatus, filter, flow and pressure tune in flowing through for hydrogen on pipeline
Save valve A, fixed bed reactors, flow and pressure-regulating valve B, product storage tank, tail gas tank, drier, connection after drier
Hydrogen gas supplying apparatus.
7. 2,5- dichloronitrobenzene uninanned platform 2 as claimed in claim 6, the device of 5- dichloroaniline, it is characterised in that:
Separately there is controller, be separately connected control flow and pressure-regulating valve A, pressure gauge, flow and pressure-regulating valve B, collect three kinds
The pressure of pressure signal and three position hydrogen of auto-control.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112479900A (en) * | 2020-11-04 | 2021-03-12 | 江苏瑞祥化工有限公司 | Method for synthesizing 2,5-dichloroaniline through kettle type continuous hydrogenation |
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