CN101607909B - Rapid material cooling and waste acid recycling process after chlorobenzene thermal insulation nitration - Google Patents
Rapid material cooling and waste acid recycling process after chlorobenzene thermal insulation nitration Download PDFInfo
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- CN101607909B CN101607909B CN2009101822873A CN200910182287A CN101607909B CN 101607909 B CN101607909 B CN 101607909B CN 2009101822873 A CN2009101822873 A CN 2009101822873A CN 200910182287 A CN200910182287 A CN 200910182287A CN 101607909 B CN101607909 B CN 101607909B
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Abstract
The invention discloses a material cooling and waste acid recycling process after chlorobenzene thermal insulation nitration, comprising the following steps of: (1) chlorobenzene nitration; (2) vacuum flashing of material after the reaction; (3) gas-liquid separation; (4) gas-phase material cooling and condensation; (5) gas-liquid separation and gas-phase material treatment; (6) liquid-liquid separation of gas-phase materials from the previous step and treatment of oil-phase materials, and the use of water-phase materials as washing water of nitrochlorobenzene crude products in the eighth step; (7) liquid-liquid separation to the liquid-phase materials obtained from gas-liquid separation in the third step, utilization of water phase for mixed acid ingredients and treatment of the oil-phase materials in a next step; (8) mixed washing of the nitrochlorobenzene crude products and the water-phase materials obtained from the liquid-liquid separation in the sixth step; and (9) further treatment of the water-phase materials obtained from the liquid-liquid separation, and further separation and refining of the oil-phase nitrochlorobenzene for obtaining the products. The rapid material cooling and waste acid recycling process after chlorobenzene thermal insulation nitration has the advantages of less three wastes, cost conservation and convenient industrial implementation.
Description
Technical field
The present invention relates to the quick cooling of material after a kind of chlorobenzene nitration reaction and the method that recovering waste acid is utilized technology, the quick cooling and the waste acid recycling process of material belong to the fine chemical technology field behind particularly a kind of chlorobenzene thermal insulation nitration.
Background technology
Nitro-chlorobenzene is mainly o-Nitrochlorobenzene, m-nitrochlorobenzene and p-Nitrophenyl chloride, and nitro-chlorobenzene is the important intermediate of industry such as dyestuff, medicine, spices.
The method that chlorobenzene thermal insulation nitration prepares nitro-chlorobenzene be with after the preheating of raw material chlorobenzene with nitration mixture in adiabatic reactor generation nitration reaction; The nitration mixture that is used for the nitration reaction process is to be mixed with certain proportion by nitric acid, sulfuric acid and water; In the chlorobenzene thermal insulation nitration process; Temperature out through nitrated reaction mass is generally 120 ℃-160 ℃, and the top hole pressure of material is 0.4MPa-0.6MPa.If the material behind the chlorobenzene thermal insulation nitration can not be lowered the temperature rapidly in a short time; Not only having a large amount of side reactions takes place; And cause the waste of energy, and sulfuric acid only uses as catalyzer in chlorobenzene and the nitric acid generation nitration reaction process, in the nitration reaction process, has water byproduct to generate.Therefore; For being lowered the temperature rapidly, reacting rear material takes place to reduce side reaction; The water byproduct that produces in the reaction process is removed rapidly; Making reacted spent acid mainly is that sulphuric acid soln is concentrated, and recycles with realization, and the energy that can make full use of reacting rear material again is a key technical problem of needing solution badly.
Characteristics to the chlorobenzene thermal insulation nitration technological process; Utilize problem in order to solve after the nitration reaction the quick cooling and the recovering waste acid of material; Provide that a kind of technical process is short, resource utilization is high, sepn process is simple, consuming little energy, process are safe and reliable, the Technology of easy operation control; The quick cooling and the recovering waste acid utilization of material after the realization nitration reaction have important use to the state of the art that promotes relevant industries and are worth.
Summary of the invention
The purpose of this invention is to provide that a kind of technical process is short, resource utilization is high, sepn process is simple, consuming little energy, process are safe and reliable, the Technology of easy operation control, solve behind the chlorobenzene thermal insulation nitration the quick cooling and the recovering waste acid of material and utilize problem.
The technical scheme that realizes above-mentioned purpose is: the cooling of material and waste acid recycling process behind a kind of chlorobenzene thermal insulation nitration, and said method steps is following:
(1) adiabatic nitration: in the thermal insulation nitration device, chlorobenzene is mixed the generation nitration reaction with nitration mixture, the nitration mixture in the nitration reaction process is to be mixed by nitric acid, sulfuric acid and water, and the material after the nitration reaction gets into next step;
(2) vacuum flashing: in vacuum flashing equipment, the material behind the last step chlorobenzene thermal insulation nitration is carried out vacuum flashing, reacted material is cooled off fast, the material after the vacuum flashing gets into next step;
(3) solution-air is separated: in the solution-air separating device, the material that a last step is obtained carries out the solution-air separation, and liquid phase is thick product of nitro-chlorobenzene and sulphuric acid soln, and goes for the 7th step further handled, and gaseous phase materials gets into next step;
(4) cooling condensation: in the cooling condensing equipment, the gaseous phase materials that a last step is obtained carries out indirect heat exchange cooling condensation, and the condensed material of lowering the temperature gets into next step;
(5) solution-air is separated: in the solution-air separating device, the material that a last step is obtained carries out the solution-air separation, and gaseous phase materials goes further off gas treatment, and liquid phase is a nitro-chlorobenzene, and gets into next step with water;
(6) liquid-liquid separation: in liquid-liquid separation equipment; The material that a last step is obtained carries out liquid-liquid separation; The oil phase chlorobenzene is as raw material recycle in the chlorobenzene thermal insulation nitration process, and the water material further utilizes as the bath water of the thick product of the 8th step nitro-chlorobenzene;
(7) liquid-liquid separation: in liquid-liquid separation equipment; The 3rd step solution-air is separated the thick product of nitro-chlorobenzene and the vitriolated waste acid water solution that obtain carry out liquid-liquid separation; The water material is as nitration mixture batching recycle in the chlorobenzene thermal insulation nitration process, and oil phase material is that the thick product of nitro-chlorobenzene goes next step processing;
(8) mixing, washing: in mixing, washing equipment, the thick product of nitro-chlorobenzene that a last step is obtained mixes with the water material that the 6th step liquid-liquid separation obtains, and blended has also played the effect of washing simultaneously, gets into next step through the material behind the mixing, washing;
(9) liquid-liquid separation: in liquid-liquid separation equipment; The material that a last step is obtained carries out liquid-liquid separation in liquid-liquid separation equipment; The water material that behind liquid-liquid separation, obtains goes further wastewater treatment, and oil phase nitro-chlorobenzene mixture goes further separation and purification to obtain o-Nitrochlorobenzene, m-nitrochlorobenzene and p-Nitrophenyl chloride product.
Further, the described vacuum flashing equipment of the second step vacuum flashing is any one in flash tank or flash cooler or the flashing tower.
The absolute pressure of further, operating in the second step vacuum flashing equipment is 0.02MPa-0.08MPa.
Further, the described cooling condensing equipment of the 4th step cooling condensation is any one in tube in-tube condenser or shell-and tube condenser or the plate-type condenser, and the temperature out of phlegma is 20 ℃-60 ℃.
Further, the 5th the step described solution-air separating device be liquid-gas separator or Sofitel air water separator.
The quick cooling of material and the principle of work of waste acid recycling process are behind the chlorobenzene thermal insulation nitration of the present invention: the material after (1) utilizes the vacuum flashing technology with chlorobenzene thermal insulation nitration is through decompression; Make its boiling point lowering; Get in the flashing apparatus; The vaporization of seething with excitement rapidly of easy volatiles water and the chlorobenzene of material in sudden strain of a muscle equipment; Remove in the system heat with the evaporation of water and chlorobenzene and get into gassy system, the material behind the chlorobenzene thermal insulation nitration is cooled fast to below 80 ℃, avoid the generation of side reaction; (2) utilize the vacuum flashing technology in evaporative process, make the raw material chlorobenzene that nitration reaction does not take place evaporate the entering gassy system with water vapor, gas phase reclaims chlorobenzene behind cooling, liquid-liquid separation; (3) make full use of the energy of the mixture heat of reaction heat and sulfuric acid and water in the chlorobenzene thermal insulation nitration process, to save the energy expenditure of process as the vacuum flashing evaporation; (4) evaporation of the water that produces in the nitrifying process is removed after; Spent acid (mainly being sulphuric acid soln) is concentrated; Liquid phase material is through liquid-liquid separation; The water spent acid is as the nitration mixture batching recycle of nitration reaction, and oil phase nitro-chlorobenzene mixture goes further separation and purification to obtain o-Nitrochlorobenzene, m-nitrochlorobenzene and p-Nitrophenyl chloride product.
Realize that the main technique equipment that the present invention needs is: vacuum flashing equipment, cooling condensing equipment, solution-air separating device and liquid-liquid separation equipment etc.
Adopt the advantage of technique scheme to be: the vacuum flashing technology is adopted in (1); The quick cooling of material behind the chlorobenzene thermal insulation nitration and the evaporation concentration of spent acid are carried out simultaneously; In same flash vaporization process, be achieved, utilize behind the chlorobenzene thermal insulation nitration evaporation of the water in the material and chlorobenzene to remove heat and get into gassy system, the material behind the chlorobenzene thermal insulation nitration is cooled fast to below 80 ℃; Avoid the generation of side reaction; Make the water that produces in the chlorobenzene thermal insulation nitration process get into gassy system simultaneously, spent acid (mainly being sulphuric acid soln) is concentrated, satisfy condition as the recycle of nitration reaction raw material; (2) adopt the vacuum flashing technology, utilize the evaporation direct heat exchange method of process water and chlorobenzene to remove behind the chlorobenzene thermal insulation nitration heat in the material, have characteristics rapidly and thoroughly; (3) in evaporating concentration process, make the raw material chlorobenzene that nitration reaction does not take place evaporate the entering gassy system with water vapor, gas phase reclaims chlorobenzene behind cooling, liquid-liquid separation; Mixture heat when (4) making full use of reaction heat and sulfuric acid in the chlorobenzene thermal insulation nitration process and mix with water is as the energy of vacuum flashing evaporation, to save the energy expenditure of process.It is few to adopt process method of the present invention to have the process quantity of three wastes, cleaning, environmental protection, and various by products can be recycled, and this has practiced thrift cost greatly, is convenient to industrializing implementation.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further detailed explanation.
Embodiment one
Main technique equipment is: thermal insulation nitration device, vacuum flashing equipment, cooling condensing equipment, solution-air separating device and liquid-liquid separation equipment etc.
As shown in Figure 1, the quick cooling and the waste acid recycling process of material behind a kind of chlorobenzene thermal insulation nitration, said process step is following:
(1) adiabatic nitration: in the adiabatic nitration static mixing reactor; The nitration mixture of nitration reaction is that 98% sulfuric acid, 65% nitric acid and water mix by a certain percentage by the massfraction of technical grade; The dehydration value of nitration mixture is 4.0, and the mol ratio of chlorobenzene and nitric acid is 1.05: 1.0, chlorobenzene is mixed with nitration mixture nitration reaction takes place; Temperature of charge after the nitration reaction is about 120 ℃, and reacted material gets into next step;
(2) vacuum flashing: the absolute working pressure in flash tank is 0.02MPa, and the material behind the last step chlorobenzene thermal insulation nitration is carried out vacuum flashing in flash tank, makes reacted material cool off about 60 ℃ fast, and the material after the vacuum flashing gets into next step;
(3) solution-air is separated: in water-and-oil separator, the material that a last step is obtained carries out the solution-air separation, and liquid phase is that thick product of nitro-chlorobenzene and sulphuric acid soln went for the 7th step further handled, and gaseous phase materials gets into next step;
(4) cooling condensation: in plate-type condenser, the gaseous phase materials that a last step is obtained carries out indirect heat exchange cooling condensation, and the temperature out of phlegma is about 20 ℃, and the condensed material of lowering the temperature gets into next step;
(5) solution-air is separated: in water-and-oil separator, the material that a last step is obtained carries out the solution-air separation, and gaseous phase materials goes further off gas treatment, oxynitride (NO in gas phase
X) content reaches and adopts method discharging in a organized way after the emission standard, liquid phase be nitro-chlorobenzene and water entering next step;
(6) liquid-liquid separation: in the decanter type liquid liquid separator; The material that a last step is obtained carries out liquid-liquid separation; The material that a last step is obtained carries out liquid-liquid separation; The oil phase chlorobenzene is as raw material recycle in the chlorobenzene thermal insulation nitration process, and the water material further utilizes as the bath water of the thick product of the 8th step nitro-chlorobenzene;
(7) liquid-liquid separation: in the decanter type liquid liquid separator; The 3rd step solution-air is separated the thick product of nitro-chlorobenzene and the vitriolated waste acid water solution that obtain carry out liquid-liquid separation; The water material is as nitration mixture batching recycle in the chlorobenzene thermal insulation nitration process, and oil phase material is that the thick product of nitro-chlorobenzene goes next step processing;
(8) mixing, washing: in the static mixing washer; Service temperature is 80 ℃; The thick product of nitro-chlorobenzene that a last step is obtained mixes with the water material that the 6th step liquid-liquid separation obtains, and blended has also played the effect of washing simultaneously, gets into next step through the material behind the mixing, washing;
(9) liquid-liquid separation: in the decanter type liquid liquid separator; The material that a last step is obtained carries out liquid-liquid separation in liquid-liquid separation equipment; The water material that behind liquid-liquid separation, obtains goes further wastewater treatment, and oil phase nitro-chlorobenzene mixture goes further separation and purification to obtain o-Nitrochlorobenzene, m-nitrochlorobenzene and p-Nitrophenyl chloride product.
Embodiment two
Main technique equipment is: thermal insulation nitration device, vacuum flashing equipment, cooling condensing equipment, solution-air separating device and liquid-liquid separation equipment etc.
As shown in Figure 1, the quick cooling and the waste acid recycling process of material behind a kind of chlorobenzene thermal insulation nitration, said process step is following:
(1) adiabatic nitration: in SV type adiabatic nitration static mixing reactor; The nitration mixture of nitration reaction is that 98% sulfuric acid, 65% nitric acid and spent acid mix by a certain percentage by the massfraction of technical grade; The dehydration value of nitration mixture is 3.0, and the mol ratio of chlorobenzene and nitric acid is 1.1: 1.0, chlorobenzene is mixed with nitration mixture nitration reaction takes place; Temperature of charge after the nitration reaction is about 140 ℃, and reacted material gets into next step;
(2) vacuum flashing: in flash cooler; At absolute working pressure is 0.04MPa; Material behind the last step chlorobenzene thermal insulation nitration is carried out vacuum flashing in flash cooler, make reacted material cool off about 70 ℃ fast, the material after the vacuum flashing gets into next step;
(3) solution-air is separated: in liquid-gas separator, the material that a last step is obtained carries out the solution-air separation, and liquid phase is that thick product of nitro-chlorobenzene and sulphuric acid soln went for the 7th step further handled, and gaseous phase materials gets into next step;
(4) cooling condensation: in shell-and tube condenser, the last gaseous phase materials that obtains of step is carried out indirect heat exchange cooling condensation, the temperature out of phlegma is about 40 ℃, and the cooling condensing equipment condensed material of lowering the temperature gets into next step;
(5) solution-air is separated: in liquid-gas separator, the material that a last step is obtained carries out the solution-air separation, and gaseous phase materials goes further off gas treatment, NO in gas phase
XContent adopts method discharging in a organized way after reaching emission standard, and liquid phase is that nitro-chlorobenzene and water get into next step;
(6) liquid-liquid separation: in centrifugal liquid liquid separator; The material that a last step is obtained carries out liquid-liquid separation; The oil phase chlorobenzene is as the raw material recycle in the chlorobenzene thermal insulation nitration process, and the water material further utilizes as the bath water of the thick product of the 8th step nitro-chlorobenzene;
(7) liquid-liquid separation: in centrifugal liquid liquid separator; The 3rd step solution-air is separated the thick product of nitro-chlorobenzene and the vitriolated waste acid water solution that obtain carry out liquid-liquid separation; The water material is as nitration mixture batching recycle in the chlorobenzene thermal insulation nitration process, and oil phase material is that the thick product of nitro-chlorobenzene goes next step processing;
(8) mixing, washing: in tubular type mixing, washing device; Service temperature is 60 ℃; The thick product of nitro-chlorobenzene that a last step is obtained mixes with the water material that the 6th step liquid-liquid separation obtains, and blended has also played the effect of washing simultaneously, gets into next step through the material behind the mixing, washing;
(9) liquid-liquid separation: in centrifugal liquid liquid separator; The material that a last step is obtained carries out liquid-liquid separation in liquid-liquid separation equipment; The water material that behind liquid-liquid separation, obtains goes further wastewater treatment, and oil phase nitro-chlorobenzene mixture goes further separation and purification to obtain o-Nitrochlorobenzene, m-nitrochlorobenzene and p-Nitrophenyl chloride product.
Embodiment three
Main technique equipment is: adiabatic nitration static mixing reactor, vacuum flashing equipment, cooling condensing equipment, solution-air separating device and liquid-liquid separation equipment etc.
As shown in Figure 1, the quick cooling and the waste acid recycling process of material behind a kind of chlorobenzene thermal insulation nitration, said process step is following:
(1) adiabatic nitration: in SV type adiabatic nitration static mixing reactor; The nitration mixture of nitration reaction is that 98% sulfuric acid, 65% nitric acid and spent acid mix by a certain percentage by the massfraction of technical grade; The dehydration value of nitration mixture is 2.0, and the mol ratio of chlorobenzene and nitric acid is 1.1: 1.0, chlorobenzene is mixed with nitration mixture nitration reaction takes place; Temperature of charge after the nitration reaction is about 160 ℃, and reacted material gets into next step;
(2) vacuum flashing: in flashing tower; Absolute working pressure in flashing tower is 0.08MPa; Material behind the last step chlorobenzene thermal insulation nitration is carried out vacuum flashing in flash tank, make reacted material cool off about 80 ℃ fast, the material after the vacuum flashing gets into next step;
(3) solution-air is separated: in the Sofitel air water separator, the material that a last step is obtained carries out the solution-air separation, and liquid phase is that thick product of nitro-chlorobenzene and sulphuric acid soln went for the 7th step further handled, and gaseous phase materials gets into next step;
(4) cooling condensation: in tube in-tube condenser, the gaseous phase materials that a last step is obtained carries out indirect heat exchange cooling condensation, and the temperature out of phlegma is about 60 ℃, and the condensed material of lowering the temperature gets into next step;
(5) solution-air is separated: in the Sofitel air water separator, the material that a last step is obtained carries out the solution-air separation, and gaseous phase materials goes further off gas treatment, NO in gas phase
XContent adopts method discharging in a organized way after reaching emission standard, and liquid phase is that nitro-chlorobenzene and water get into next step;
(6) liquid-liquid separation: in efficient oil-water separator; The material that a last step is obtained carries out liquid-liquid separation; The oil phase chlorobenzene is as raw material recycle in the chlorobenzene thermal insulation nitration process, and the water material further utilizes as the bath water of the thick product of the 8th step nitro-chlorobenzene;
(7) liquid-liquid separation: in efficient oil-water separator; The material that a last step is obtained carries out liquid-liquid separation; The 3rd step solution-air is separated the thick product of nitro-chlorobenzene and the vitriolated waste acid water solution that obtain carry out liquid-liquid separation; The water material is as nitration mixture batching recycle in the chlorobenzene thermal insulation nitration process, and oil phase material is that the thick product of nitro-chlorobenzene goes next step processing;
(8) mixing, washing: mix in the washer in the still formula; The mixing, washing service temperature is 80 ℃; The thick product of nitro-chlorobenzene that a last step is obtained mixes with the water material that the 6th step liquid-liquid separation obtains; Blended has also played the effect of washing simultaneously, gets into next step through the material behind the mixing, washing;
(9) liquid-liquid separation: in efficient oil-water separator; The material that a last step is obtained carries out liquid-liquid separation in liquid-liquid separation equipment; The water material that behind liquid-liquid separation, obtains goes further wastewater treatment, and oil phase nitro-chlorobenzene mixture goes further separation and purification to obtain o-Nitrochlorobenzene, m-nitrochlorobenzene and p-Nitrophenyl chloride product.
Remove the various embodiments described above, embodiment of the present invention also have a lot, and the technical scheme that all employings are equal to or equivalence is replaced is all within protection scope of the present invention.
Claims (5)
1. the cooling and the waste acid recycling process of material behind the chlorobenzene thermal insulation nitration is characterized in that said method steps is following:
(1) adiabatic nitration: in the thermal insulation nitration device, chlorobenzene is mixed the generation nitration reaction with nitration mixture, the nitration mixture in the nitration reaction process is to be mixed by nitric acid, sulfuric acid and water, and the material after the nitration reaction gets into next step;
(2) vacuum flashing: in vacuum flashing equipment, the material behind the last step chlorobenzene thermal insulation nitration is carried out vacuum flashing, reacted material is cooled off fast, the material after the vacuum flashing gets into next step;
(3) solution-air is separated: in the solution-air separating device, the material that a last step is obtained carries out the solution-air separation, and liquid phase is thick product of nitro-chlorobenzene and sulphuric acid soln, and goes for the 7th step further handled, and gaseous phase materials gets into next step;
(4) cooling condensation: in the cooling condensing equipment, the gaseous phase materials that a last step is obtained carries out indirect heat exchange cooling condensation, and the condensed material of lowering the temperature gets into next step;
(5) solution-air is separated: in the solution-air separating device, the material that a last step is obtained carries out the solution-air separation, and gaseous phase materials goes further off gas treatment, and liquid phase is a nitro-chlorobenzene, and gets into next step with water;
(6) liquid-liquid separation: in liquid-liquid separation equipment; The material that a last step is obtained carries out liquid-liquid separation; The oil phase chlorobenzene is as raw material recycle in the chlorobenzene thermal insulation nitration process, and the water material further utilizes as the bath water of the thick product of the 8th step nitro-chlorobenzene;
(7) liquid-liquid separation: in liquid-liquid separation equipment; The 3rd step solution-air is separated the thick product of nitro-chlorobenzene and the vitriolated waste acid water solution that obtain carry out liquid-liquid separation; The water material is as nitration mixture batching recycle in the chlorobenzene thermal insulation nitration process, and oil phase material is that the thick product of nitro-chlorobenzene goes next step processing;
(8) mixing, washing: in mixing, washing equipment, the thick product of nitro-chlorobenzene that a last step is obtained mixes with the water material that the 6th step liquid-liquid separation obtains, and blended has also played the effect of washing simultaneously, gets into next step through the material behind the mixing, washing;
(9) liquid-liquid separation: in liquid-liquid separation equipment; The material that a last step is obtained carries out liquid-liquid separation in liquid-liquid separation equipment; The water material that behind liquid-liquid separation, obtains goes further wastewater treatment, and oil phase nitro-chlorobenzene mixture goes further separation and purification to obtain o-Nitrochlorobenzene, m-nitrochlorobenzene and p-Nitrophenyl chloride product.
2. the cooling and the waste acid recycling process of material behind a kind of chlorobenzene thermal insulation nitration according to claim 1 is characterized in that: the described vacuum flashing equipment of the second step vacuum flashing is any one in flash tank or flash cooler or the flashing tower.
3. the cooling and the waste acid recycling process of material behind a kind of chlorobenzene thermal insulation nitration according to claim 1 is characterized in that: the absolute pressure of operating in the second step vacuum flashing equipment is 0.02MPa-0.08MPa.
4. the cooling and the waste acid recycling process of material behind a kind of chlorobenzene thermal insulation nitration according to claim 1; It is characterized in that: the described cooling condensing equipment of the 4th step cooling condensation is any one of tube in-tube condenser or shell-and tube condenser or plate-type condenser, and the temperature out of phlegma is 20 ℃-60 ℃.
5. the cooling and the waste acid recycling process of material behind a kind of chlorobenzene thermal insulation nitration according to claim 1 is characterized in that: the 5th step, described solution-air separating device was liquid-gas separator or Sofitel air water separator.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102234233A (en) * | 2010-04-20 | 2011-11-09 | 安徽八一化工股份有限公司 | Method for extracting organic matters from waste acid during nitrochlorobenzene production |
| CN102390820A (en) * | 2011-08-17 | 2012-03-28 | 中国石油化工股份有限公司 | Method for reclaiming nitric acid from nitrified waste acid |
| CN103214388B (en) * | 2012-01-20 | 2015-08-26 | 浙江龙盛化工研究有限公司 | A kind of recoverying and utilizing method of nitrating wasting acid |
| CN103382155B (en) * | 2013-05-21 | 2015-03-25 | 浙江康峰化工有限公司 | Method for recovering organic matters in nitrifying waste acid |
| CN103980126A (en) * | 2014-05-12 | 2014-08-13 | 中石化南京工程有限公司 | Separation method of nitrochlorobenzene |
| CN104707430B (en) * | 2015-03-04 | 2016-08-10 | 中国石油化工股份有限公司青岛安全工程研究院 | Chloronitrobenzene emission-control equipment during tank car entrucking |
| CN112707823B (en) * | 2020-12-30 | 2022-02-18 | 东营安诺其纺织材料有限公司 | Green, safe, efficient and continuous 2, 4-dinitrochlorobenzene production system and method |
| CN113072450A (en) * | 2021-04-07 | 2021-07-06 | 中北大学 | Preparation method of m-nitrochlorobenzene |
| CN113998824B (en) * | 2021-10-11 | 2023-08-29 | 金能科技股份有限公司 | Production method and equipment for reducing salt content and solid waste of p-methylphenol |
| CN114539063A (en) * | 2022-02-11 | 2022-05-27 | 安徽东至广信农化有限公司 | Method for producing nitrochlorobenzene by vacuum concentration method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4021498A (en) * | 1975-12-09 | 1977-05-03 | American Cyanamid Company | Adiabatic process for nitration of nitratable aromatic compounds |
| US4453027A (en) * | 1982-12-10 | 1984-06-05 | Monsanto Company | Adiabatic process for the nitration of halobenzenes |
| EP0675104A1 (en) * | 1994-03-30 | 1995-10-04 | Bayer Ag | Process for adiabatic preparation of mononitrohalogenbenzenes |
| CN1133283A (en) * | 1995-10-20 | 1996-10-16 | 清华大学 | Preparing nitro-chlorobenzene by catalytic nitration |
-
2009
- 2009-07-07 CN CN2009101822873A patent/CN101607909B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4021498A (en) * | 1975-12-09 | 1977-05-03 | American Cyanamid Company | Adiabatic process for nitration of nitratable aromatic compounds |
| US4453027A (en) * | 1982-12-10 | 1984-06-05 | Monsanto Company | Adiabatic process for the nitration of halobenzenes |
| EP0675104A1 (en) * | 1994-03-30 | 1995-10-04 | Bayer Ag | Process for adiabatic preparation of mononitrohalogenbenzenes |
| CN1133283A (en) * | 1995-10-20 | 1996-10-16 | 清华大学 | Preparing nitro-chlorobenzene by catalytic nitration |
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