CN106883129A - A kind of method that utilization meta oil prepares m-chloroaniline - Google Patents
A kind of method that utilization meta oil prepares m-chloroaniline Download PDFInfo
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- CN106883129A CN106883129A CN201611246576.1A CN201611246576A CN106883129A CN 106883129 A CN106883129 A CN 106883129A CN 201611246576 A CN201611246576 A CN 201611246576A CN 106883129 A CN106883129 A CN 106883129A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/30—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds
- C07C209/32—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups
- C07C209/36—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups by reduction of nitro groups bound to carbon atoms of six-membered aromatic rings in presence of hydrogen-containing gases and a catalyst
- C07C209/365—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups by reduction of nitro groups bound to carbon atoms of six-membered aromatic rings in presence of hydrogen-containing gases and a catalyst by reduction with preservation of halogen-atoms in compounds containing nitro groups and halogen atoms bound to the same carbon skeleton
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/12—Preparation of nitro compounds by reactions not involving the formation of nitro groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/16—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/02—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions involving the formation of amino groups from compounds containing hydroxy groups or etherified or esterified hydroxy groups
Abstract
The present invention relates to a kind of method that utilization meta oil prepares m-chloroaniline, belong to the preparing technical field of m-chloroaniline, specifically include the steps such as dispensing reaction, washing, drying, three-level vacuum distillation, crystallization, reduction, redistillation.The present invention is to be raw material to, the waste material meta oil of adjacent nitre production and industrial wastes NaHS, using methoxylation, crystallization and reduction, prepare m-chloroaniline, and generate accessory substance o-aminoanisole and paraphenetidine, so as to realize low cost, high production, than existing production technology, there is obvious cost advantage, with economic benefit higher.
Description
Technical field
The invention belongs to the preparing technical field of m-chloroaniline, m-chloroaniline is prepared using meta oil more particularly, to one kind
Method.
Background technology
M-chloroaniline, colourless liquid is poisonous to light amber liquid, is a kind of important fine-chemical intermediate, mainly
Intermediate, medicine, insecticide as azo dyes and pigment, chemistry of pesticide product.
Meta oil, main component be between, adjacent, parachloronitrobenzene, be in adjacent nitre production technology to two kinds of products of nitre and adjacent nitre
Product and the general name rich in m-chloronitrobenzene and high boiling point organic compound waste liquid.
The existing method for preparing m-chloroaniline is that m-chloronitrobenzene is carried out into nitro reduction to prepare m-chloroaniline mostly.
Traditional nitro reduction mainly has iron powder reducing method, sodium sulfide reducing method, catalytic hydrogenating reduction method, electrochemical reducing.Iron powder
Reducing process produces a large amount of iron cements, severe contamination environment；There is reduction route complexity in sodium sulfide reducing method, product yield is low, waste liquid
The features such as measuring big；Electrochemical reducing energy consumption is too high；Catalytic hydrogenation method has reaction scheme, and energy consumption is low, advantages of environment protection, but
It is, in m-chloronitrobenzene catalytic hydrogenation, because the meta activation of nitro can also increase the dechlorination life of generation C-CL key hydrogenolysis
Into the side reaction of aniline, so as to reduce the yield of principal product.Meanwhile, the hydrogen chloride of dechlorination generation can also cause corruption to equipment
Erosion.
In sum, at present, there is raw material m-chloronitrobenzene high cost, the pollution of auxiliary material iron powder reducing in prior art
The problems such as environment, vulcanized sodium reduction high cost, the easy dechlorination of hydro-reduction, etching apparatus.
The content of the invention
In order to solve the above-mentioned technical problem, the present invention provides a kind of oily as raw material with meta cheap and easy to get, prepares m-chloro
The method of aniline, this method has the characteristics of rate of recovery high, low cost, suitable large-scale production.
In order to realize the purpose of the present invention, adopt the following technical scheme that：
A kind of method that utilization meta oil prepares m-chloroaniline, comprises the following steps：
(1) dispensing reaction：Meta oil is added in methoxylation kettle, is measured from methyl alcohol measuring tank under air-tight state
Methyl alcohol is added, then puts into catalyst ammonium chloride, stirred, while heating response kettle temperature degree is to 58-63 DEG C, adjust the pressure of reactor
It is 0-0.2MPa, NaOH is added in most backward reactor, keeping temperature is constant, detection is sampled after reaction 5h；Wherein, meta
Oil：Methyl alcohol：NaOH：Mass ratio=1 of ammonium chloride：0.30：0.32：0.045, when detect paranitrochlorobenzene content≤
0.1% and during o-nitrochlorobenzene content≤2%, methyl alcohol is reclaimed, then it is transferred to down one washing step；
(2) wash：The material pump that step (1) reaction is obtained is delivered to workshop and deposits tank, then material is deposited from workshop
Washing kettle washing is squeezed into tank, the amount of squeezing into of material is 2/3rds of washing kettle volume, then by washing twice, each water
The addition of wash water is a quarter of the material amount of squeezing into, and stirs 0.5h, then stand 2h；Waste water feeding waste water tank after washing,
Enter dry preceding tank by the material after washing；
(3) dry：Vavuum pump is opened, opening receives water pot vacuum valve and condenser water valve, and opening takes out material valve from dry preceding tank
It is pumped into the material after washing and enters dehydrating kettle, it is 2/3rds of dehydrating kettle volume to be pumped into the amount of material, is then stirred, crack steaming
Vapour is dehydrated, and when substantially anhydrous in condenser visor, terminates dehydration, is then shut off vacuum valve and air outlet valve, opens pneumatics
By in the dry rear tank of dried material press-in；
(4) rectifying：It is evaporated in vacuo using three-level, to separate m-chloro-nitrobenzene, and removes a small amount of Benzene Chloride, detailed process is such as
Under：
1# towers：Step (3) dried material is introduced to 1# towers, and is heated up simultaneously, when bottom temperature rises to 100 DEG C
When, vavuum pump is opened, 1# towers, 2# towers and 3# towers are all evacuated to -0.096Mpa, while opening water circulating pump, adjusting tower
The Inlet and outlet water of condenser is pushed up, when tower top temperature is 50-60 DEG C, infinite reflux 2-3h makes to start extraction after reaching balance in tower, adjusts
Section 1# bottom temperatures are 145-155 DEG C, and pressure is -0.1Mpa, from overhead collection low-boiling-point substance, the material in tower reactor is continuously pumped into
To in 2# towers；
2# towers：Material in 1# tower reactors is continuously pumped into 2# tower middle charging apertures, regulation 2# bottom temperatures are 170-180
DEG C, pressure is -0.1Mpa, and m-chloro-nitrobenzene is isolated from tower top, and its content >=90% is then fed into crystallization kettle；By 2# tower reactors
Interior material is continuously pumped into 3# towers, and this process keeps inlet amount and extraction doses balance, and volume of material is all the time in making tower reactor
It is one of three of tower reactor volume；
3# towers：Material in 2# tower reactors is continuously pumped into 3# towers, regulation 3# bottom temperatures are 170-180 DEG C, pressure
It is -0.1Mpa, Nitroanisole is separated from tower reactor, put No. 1 intermediate storage tank into, carries out subsequent treatment；The circulation of tower top material is continuous
Pump into 2# tower middle charging apertures；
(5) crystallize：The m-chloro-nitrobenzene pump that 2# towers are separated is squeezed into crystallization kettle, when flow back visor in have backflow
Termination of pumping afterwards, opens circulating pump, and to crystallization kettle fast cooling, after temperature is down to 45 DEG C, regulation circulating pump water valve is slowly dropped
Temperature, when temperature is less than 27 DEG C, crystallization is completed, and then detects the content of m-chloro-nitrobenzene；When m-chloro-nitrobenzene content >=
99.5%, m-chloro-nitrobenzene is pumped into No. 2 intermediate storage tanks, sold outside m-chloroaniline or directly packaging for follow-up preparation；M-chloro nitro
Between 93%~99.5%, crystallization again is used benzene content；It is unified to collect when m-chloro-nitrobenzene content is less than 93%, will
It pumps into the 2# further rectification and purifications of tower middle charging aperture；
(6) reduce：By in the sodium hydrosulfide aqueous solution addition reduction kettle of 350g/L, the temperature of reduction kettle is gradually risen extremely
110 DEG C, then by measuring tank to adding No. 2 m-chloro-nitrobenzenes of intermediate storage tank in reactor, then adjust temperature in the kettle and be
135-145 DEG C, pressure is 0.25Mpa, and reduction reaction occurs with NaHS, and reaction terminates rear stratification, and lower floor is water, sulphur
The mixture of sodium thiosulfate, NaHS and NaOH, by pipeline to dodium thiosulfate preparation section, the reduction of upper strata crude product
Material sends into amino tank, for subsequent processing；Wherein m-chloro-nitrobenzene：Mass ratio=3 of NaHS:5.5；
(7) distill：Crude product reducing material in amino tank is incorporated into distillation still, kettle temperature is raised to 170 DEG C, through vacuum
Water and trace impurity in distillation removal crude product reducing material, obtain finished product m-chloroaniline, and bottom material is drawn and carried out at solid waste
Reason.
Preferably, the temperature washed twice in step (2) is 65-70 DEG C.
Preferably, the speed of agitator in step (1) and step (2) is 60r/min.
Further, the material that step (1) reaction is obtained includes paranitroanisole, ortho-nitroanisole, m-chloro nitro
Benzene, water, Sodium p-nitrophenoxide, sodium onitrophenol, sodium chloride and low-boiling-point substance.
Preferably, the pressure of dehydrating kettle is -0.1-0Mpa, and temperature is higher than 85 DEG C.
Further, low-boiling-point substance is the chlorobenzene of nitrobenzene, water and content less than 1%.
The Nitroanisole in No. 1 intermediate storage tank further can also react with sodium hydrosulfide in the present invention, so
After distilled, obtain aminoanisole, and then carry out rectifying obtaining byproduct o-aminoanisole and paraphenetidine.
Compared with prior art, beneficial effects of the present invention：
The present invention to be raw material to, the waste material meta oil of adjacent nitre production and industrial wastes NaHS, using methoxylation,
Crystallization and reduction, prepare m-chloroaniline, and generate accessory substance o-aminoanisole and paraphenetidine, so as to realize it is low into
Originally, high production, than existing production technology, there is obvious cost advantage, with economic benefit higher.
Specific embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out under premised on technical solution of the present invention
Implement, give detailed implementation method and specific operating process, but protection scope of the present invention is not limited to following implementations
Example.
Embodiment
A kind of method that utilization meta oil prepares m-chloroaniline, comprises the following steps：
(1) dispensing reaction：Meta oil is added in methoxylation kettle, is measured from methyl alcohol measuring tank under air-tight state
Methyl alcohol is added, then puts into catalyst ammonium chloride, stirred, rotating speed is 60r/min, while heating response kettle temperature degree is to 58-63 DEG C, adjusted
The pressure for saving reactor is that NaOH is added in 0-0.2MPa, most backward reactor, and keeping temperature is constant, is sampled after reaction 5h
Detection；Wherein, meta oil：Methyl alcohol：NaOH：Mass ratio=1 of ammonium chloride：0.30：0.32：0.045, when detecting to nitre
When base chlorobenzene content≤0.1% and o-nitrochlorobenzene content≤2%, methyl alcohol is reclaimed, be then transferred to down one washing step；
(2) wash：The material pump that step (1) reaction is obtained is delivered to workshop and deposits tank, the material includes p-nitrophenyl
Methyl ether, ortho-nitroanisole, m-chloro-nitrobenzene, water, Sodium p-nitrophenoxide, sodium onitrophenol, sodium chloride and low-boiling-point substance, then
Material is deposited from workshop and squeezed into tank washing kettle washing, the amount of squeezing into of material is 2/3rds of washing kettle volume, is then passed through
Wash twice, the addition of each washing water is a quarter of the material amount of squeezing into, stir 0.5h, rotating speed is 60r/min, then quiet
2h is put, the temperature washed twice is 65-70 DEG C；Waste water feeding waste water tank after washing, before the material after washing enters and does
Tank；
(3) dry：Vavuum pump is opened, opening receives water pot vacuum valve and condenser water valve, and opening takes out material valve from dry preceding tank
It is pumped into the material after washing and enters dehydrating kettle, it is 2/3rds of dehydrating kettle volume to be pumped into the amount of material, adjusts the pressure of dehydrating kettle
Power is -0.1-0Mpa, and temperature is higher than 85 DEG C, is then stirred, and crack steam is dehydrated, when substantially anhydrous in condenser visor
When, terminate dehydration, vacuum valve and air outlet valve are then shut off, be pressed into for dried material after doing in tank by opening pneumatics；
(4) rectifying：It is evaporated in vacuo using three-level, to separate m-chloro-nitrobenzene, and removes a small amount of Benzene Chloride, detailed process is such as
Under：
1# towers：Step (3) dried material is introduced to 1# towers, and is heated up simultaneously, when bottom temperature rises to 100 DEG C
When, vavuum pump is opened, 1# towers, 2# towers and 3# towers are all evacuated to -0.096Mpa, while opening water circulating pump, adjusting tower
The Inlet and outlet water of condenser is pushed up, when tower top temperature is 50-60 DEG C, infinite reflux 2-3h makes to start extraction after reaching balance in tower, adjusts
Section 1# bottom temperatures are 145-155 DEG C, and pressure is -0.1Mpa, and from overhead collection low-boiling-point substance, low-boiling-point substance is nitrobenzene, water and contains
Chlorobenzene of the amount less than 1%, the material in tower reactor is continuously pumped into 2# towers；
2# towers：Material in 1# tower reactors is continuously pumped into 2# tower middle charging apertures, regulation 2# bottom temperatures are 170-180
DEG C, pressure is -0.1Mpa, and m-chloro-nitrobenzene is isolated from tower top, and its content >=90% is then fed into crystallization kettle；By 2# tower reactors
Interior material is continuously pumped into 3# towers, and this process keeps inlet amount and extraction doses balance, and volume of material is all the time in making tower reactor
It is one of three of tower reactor volume；
3# towers：Material in 2# tower reactors is continuously pumped into 3# towers, regulation 3# bottom temperatures are 170-180 DEG C, pressure
It is -0.1Mpa, Nitroanisole is separated from tower reactor, put No. 1 intermediate storage tank into, carries out subsequent treatment；The circulation of tower top material is continuous
Pump into 2# tower middle charging apertures；
(5) crystallize：The m-chloro-nitrobenzene pump that 2# towers are separated is squeezed into crystallization kettle, when flow back visor in have backflow
Termination of pumping afterwards, opens circulating pump, and to crystallization kettle fast cooling, after temperature is down to 45 DEG C, regulation circulating pump water valve is slowly dropped
Temperature, when temperature is less than 27 DEG C, crystallization is completed, and then detects the content of m-chloro-nitrobenzene；When m-chloro-nitrobenzene content >=
99.5%, m-chloro-nitrobenzene is pumped into No. 2 intermediate storage tanks, sold outside m-chloroaniline or directly packaging for follow-up preparation；M-chloro nitro
Between 93%~99.5%, crystallization again is used benzene content；It is unified to collect when m-chloro-nitrobenzene content is less than 93%, will
It pumps into the 2# further rectification and purifications of tower middle charging aperture；
(6) reduce：By in the sodium hydrosulfide aqueous solution addition reduction kettle of 350g/L, the temperature of reduction kettle is gradually risen extremely
110 DEG C, then by measuring tank to adding No. 2 m-chloro-nitrobenzenes of intermediate storage tank in reactor, then adjust temperature in the kettle and be
135-145 DEG C, pressure is 0.25Mpa, and reduction reaction occurs with NaHS, and reaction terminates rear stratification, and lower floor is water, sulphur
The mixture of sodium thiosulfate, NaHS and NaOH, by pipeline to dodium thiosulfate preparation section, the reduction of upper strata crude product
Material sends into amino tank, for subsequent processing；Wherein m-chloro-nitrobenzene：Mass ratio=3 of NaHS:5.5；
(7) distill：Crude product reducing material in amino tank is incorporated into distillation still, kettle temperature is raised to 170 DEG C, through vacuum
Water and trace impurity in distillation removal crude product reducing material, obtain finished product m-chloroaniline, and bottom material is drawn and carried out at solid waste
Reason.
In the present invention, the Nitroanisole in No. 1 intermediate storage tank can be incorporated into reduction kettle by measuring tank, also
The sodium hydrosulfide of 350g/L, the Nitroanisole of addition are added in former kettle：Mass ratio=3 of NaHS:5.5, regulation
The temperature of reduction kettle is 140 DEG C, and pressure is 0.25Mpa, Nitroanisole is reacted with sodium hydrosulfide, and reaction terminates rear quiet
Layering is put, upper materials are sent into 170 DEG C of distillation still, water and trace impurity are removed by vacuum distillation, obtain aminobenzene
Methyl ether, then aminoanisole is carried out into rectifying, obtain byproduct o-aminoanisole and paraphenetidine.
The present invention using methoxylation, is crystallized and reduction, system with waste material meta oil and industrial wastes NaHS as raw material
It is standby go out m-chloroaniline, and produce accessory substance o-aminoanisole and paraphenetidine, so as to realize low cost, high production, than
Existing production technology, there is obvious cost advantage, with economic benefit higher.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (6)
1. a kind of method that utilization meta oil prepares m-chloroaniline, it is characterised in that comprise the following steps：
(1) dispensing reaction：Meta oil is added in methoxylation kettle, it is metered from methyl alcohol measuring tank under air-tight state
Methyl alcohol, then catalyst ammonium chloride is put into, stir, while heating response kettle temperature degree is to 58-63 DEG C, the pressure for adjusting reactor is 0-
NaOH is added in 0.2MPa, most backward reactor, keeping temperature is constant, detection is sampled after reaction 5h；Wherein, meta oil：
Methyl alcohol：NaOH：Mass ratio=1 of ammonium chloride：0.30：0.32：0.045, when detecting paranitrochlorobenzene content≤0.1%
And during o-nitrochlorobenzene content≤2%, methyl alcohol is reclaimed, then it is transferred to down one washing step；
(2) wash：The material pump that step (1) reaction is obtained is delivered to workshop and deposits tank, then material is deposited in tank from workshop
Washing kettle washing is squeezed into, the amount of squeezing into of material is 2/3rds of washing kettle volume, then by washing twice, each washing water
Addition be a quarter of the material amount of squeezing into, stir 0.5h, then stand 2h；Waste water feeding waste water tank after washing, passes through
Material after washing enters dry preceding tank；
(3) dry：Vavuum pump is opened, opening receives water pot vacuum valve and condenser water valve, and opening is taken out material valve and is pumped into from dry preceding tank
Material after washing enters dehydrating kettle, and it is 2/3rds of dehydrating kettle volume to be pumped into the amount of material, is then stirred, and crack steam enters
Row dehydration, when substantially anhydrous in condenser visor, terminates dehydration, is then shut off vacuum valve and air outlet valve, and opening pneumatics will be dry
In the dry rear tank of material press-in after dry；
(4) rectifying：It is evaporated in vacuo using three-level, to separate m-chloro-nitrobenzene, and removes a small amount of Benzene Chloride, detailed process is as follows：
1# towers：Step (3) dried material is introduced to 1# towers, and is heated up simultaneously, when bottom temperature rises to 100 DEG C,
Vavuum pump is opened, 1# towers, 2# towers and 3# towers are all evacuated to -0.096Mpa, while opening water circulating pump, regulation tower top is cold
The Inlet and outlet water of condenser, when tower top temperature is 50-60 DEG C, infinite reflux 2-3h makes to start extraction after reaching balance in tower, adjusts 1#
Bottom temperature is 145-155 DEG C, and pressure is -0.1Mpa, from overhead collection low-boiling-point substance, the material in tower reactor is continuously pumped into 2#
In tower；
2# towers：Material in 1# tower reactors is continuously pumped into 2# tower middle charging apertures, regulation 2# bottom temperatures are 170-180 DEG C, pressure
Power is -0.1Mpa, and m-chloro-nitrobenzene is isolated from tower top, and its content >=90% is then fed into crystallization kettle；By the thing in 2# tower reactors
Material is continuously pumped into 3# towers, and this process keeps inlet amount and extraction doses balance, and volume of material is always tower reactor in making tower reactor
One of three of volume；
3# towers：Material in 2# tower reactors is continuously pumped into 3# towers, regulation 3# bottom temperatures are 170-180 DEG C, pressure for-
0.1Mpa, Nitroanisole is separated from tower reactor, puts No. 1 intermediate storage tank into, carries out subsequent treatment；The circulation of tower top material is continuously pumped into
2# tower middle charging apertures；
(5) crystallize：The m-chloro-nitrobenzene pump that 2# towers are separated is squeezed into crystallization kettle, is stopped after having backflow in the visor that flows back
Pump, opens circulating pump, and to crystallization kettle fast cooling, after temperature is down to 45 DEG C, regulation circulating pump water valve carries out slow cooling, when
When temperature is less than 27 DEG C, crystallization is completed, and then detects the content of m-chloro-nitrobenzene；When content >=99.5% of m-chloro-nitrobenzene,
M-chloro-nitrobenzene is pumped into No. 2 intermediate storage tanks, is sold outside m-chloroaniline or directly packaging for follow-up preparation；M-chloro-nitrobenzene content exists
Between 93%~99.5%, crystallization again is used；It is unified to collect when m-chloro-nitrobenzene content is less than 93%, it is pumped into 2#
The further rectification and purification of tower middle charging aperture；
(6) reduce：By in the sodium hydrosulfide aqueous solution addition reduction kettle of 350g/L, the temperature of reduction kettle is gradually risen to 110 DEG C,
Then by measuring tank to No. 2 m-chloro-nitrobenzenes of intermediate storage tank of addition in reactor, then temperature in the kettle is adjusted for 135-145
DEG C, pressure is 0.25Mpa, and reduction reaction occurs with NaHS, and reaction terminates rear stratification, and lower floor is water, thiosulfuric acid
The mixture of sodium, NaHS and NaOH, by pipeline to dodium thiosulfate preparation section, upper strata crude product reducing material is sent
Enter amino tank, for subsequent processing；Wherein m-chloro-nitrobenzene：Mass ratio=3 of NaHS:5.5；
(7) distill：Crude product reducing material in amino tank is incorporated into distillation still, kettle temperature is raised to 170 DEG C, through vacuum distillation
Water and trace impurity in removal crude product reducing material, obtain finished product m-chloroaniline, and bottom material is drawn and carries out fixed-end forces.
2. the method that a kind of utilization meta oil according to claim 1 prepares m-chloroaniline, it is characterised in that step (2)
In the temperature washed twice be 65-70 DEG C.
3. the method that a kind of utilization meta oil according to claim 1 prepares m-chloroaniline, it is characterised in that step (1)
It is 60r/min with the speed of agitator in step (2).
4. the method that a kind of utilization meta oil according to claim 1 prepares m-chloroaniline, it is characterised in that step (1)
The material that reaction is obtained includes paranitroanisole, ortho-nitroanisole, m-chloro-nitrobenzene, water, Sodium p-nitrophenoxide, adjacent nitro
Sodium phenate, sodium chloride and low-boiling-point substance.
5. the method that a kind of utilization meta oil according to claim 1 prepares m-chloroaniline, it is characterised in that dehydrating kettle
Pressure is -0.1-0Mpa, and temperature is higher than 85 DEG C.
6. the method that a kind of utilization meta oil according to claim 1 prepares m-chloroaniline, it is characterised in that low-boiling-point substance is
The chlorobenzene of nitrobenzene, water and content less than 1%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109369409A (en) * | 2018-11-09 | 2019-02-22 | 宁夏华御化工有限公司 | Nitro-chlorobenzene produces interposition oil separation reutilization system and meta position oil separating method |
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