CN101602561B - Process for comprehensive use and treatment of wastewater from chlorobenzene adiabatic nitration material separation - Google Patents
Process for comprehensive use and treatment of wastewater from chlorobenzene adiabatic nitration material separation Download PDFInfo
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- CN101602561B CN101602561B CN2009101822892A CN200910182289A CN101602561B CN 101602561 B CN101602561 B CN 101602561B CN 2009101822892 A CN2009101822892 A CN 2009101822892A CN 200910182289 A CN200910182289 A CN 200910182289A CN 101602561 B CN101602561 B CN 101602561B
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- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 title claims abstract description 136
- 239000000463 material Substances 0.000 title claims abstract description 112
- 238000000926 separation method Methods 0.000 title claims abstract description 94
- 239000002351 wastewater Substances 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 61
- 238000006396 nitration reaction Methods 0.000 title claims abstract description 54
- 239000007788 liquid Substances 0.000 claims abstract description 92
- 238000000605 extraction Methods 0.000 claims abstract description 52
- 239000012071 phase Substances 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- BFCFYVKQTRLZHA-UHFFFAOYSA-N 1-chloro-2-nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1Cl BFCFYVKQTRLZHA-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000005406 washing Methods 0.000 claims abstract description 35
- 239000000047 product Substances 0.000 claims abstract description 30
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 239000007791 liquid phase Substances 0.000 claims abstract description 14
- 238000009833 condensation Methods 0.000 claims abstract description 12
- 230000005494 condensation Effects 0.000 claims abstract description 12
- 239000007790 solid phase Substances 0.000 claims abstract description 6
- 238000009270 solid waste treatment Methods 0.000 claims abstract 2
- 238000001179 sorption measurement Methods 0.000 claims description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 230000003068 static effect Effects 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- KMAQZIILEGKYQZ-UHFFFAOYSA-N 1-chloro-3-nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC(Cl)=C1 KMAQZIILEGKYQZ-UHFFFAOYSA-N 0.000 claims description 7
- CZGCEKJOLUNIFY-UHFFFAOYSA-N 4-Chloronitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C=C1 CZGCEKJOLUNIFY-UHFFFAOYSA-N 0.000 claims description 7
- 239000010865 sewage Substances 0.000 claims description 6
- 239000010881 fly ash Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003463 adsorbent Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 claims description 2
- 239000002808 molecular sieve Substances 0.000 claims description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- 230000006837 decompression Effects 0.000 claims 4
- 238000001704 evaporation Methods 0.000 claims 4
- 230000008020 evaporation Effects 0.000 claims 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- 239000012043 crude product Substances 0.000 claims 3
- 239000008346 aqueous phase Substances 0.000 claims 2
- 239000005416 organic matter Substances 0.000 claims 2
- 238000004062 sedimentation Methods 0.000 claims 2
- 239000005909 Kieselgur Substances 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 claims 1
- JMDZDJNPYFJBEX-UHFFFAOYSA-N chlorobenzene;1-chloro-2-nitrobenzene Chemical compound ClC1=CC=CC=C1.[O-][N+](=O)C1=CC=CC=C1Cl JMDZDJNPYFJBEX-UHFFFAOYSA-N 0.000 claims 1
- HSSFHZJIMRUXDM-UHFFFAOYSA-N hydroxy(oxo)azanium chloride Chemical compound Cl.[O-][NH+]=O HSSFHZJIMRUXDM-UHFFFAOYSA-N 0.000 claims 1
- 239000006227 byproduct Substances 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract 1
- 238000009413 insulation Methods 0.000 description 26
- 238000005516 engineering process Methods 0.000 description 8
- 239000007792 gaseous phase Substances 0.000 description 8
- 239000002594 sorbent Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 239000002910 solid waste Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000004065 wastewater treatment Methods 0.000 description 3
- 239000012074 organic phase Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000003851 biochemical process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000010883 coal ash Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000007701 flash-distillation Methods 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000001546 nitrifying effect Effects 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a process for the comprehensive use and treatment of wastewater from chlorobenzene adiabatic nitration material separation, which comprises the following steps: (1) vacuum flashing; (2) gas-liquid separation, during which a liquid phase material undergoes liquid-liquid separation to give a coarse product of nitrochlorobenzene and a gas phase material goes to the next step; (3) temperature reduction and condensation; (4) liquid-liquid separation, during which an chlorobenzene oil phase material is recovered for use and a water phase material goes to the next step; (5) mixing and washing, during which a water phase material and the coarse product of nitrochlorobenzene are mixed and are washed at the same time; (6), liquid-liquid separation, during which an oil phase which is the coarse product of nitrochlorobenzene is subjected to further treatment and a water phase material goes to the next step; (7) extraction and separation; (8) liquid-liquid separation, during which a waste water raffinate phase goes to the next step; (9) deep removal of organisms in waste water by an absorption method; and (10) solid-liquid separation, during which a solid phase material is subjected to solid waste treatment. The process has the advantages of small waste water amount, good side product recycling, low treatment cost and convenient industrial implementation.
Description
Technical field
The present invention relates to the comprehensive utilization and the treatment process of waste water in a kind of chlorobenzene thermal insulation nitration feed separation process, belong to fine chemical technology and technical field of waste water processing.
Background technology
The process that chlorobenzene thermal insulation nitration prepares nitro-chlorobenzene be with after the preheating of raw material chlorobenzene with nitration mixture in thermal insulation nitration device generation nitration reaction, the nitration mixture that is used for nitration reaction is mixed with certain proportion by nitric acid, sulfuric acid and water, has water byproduct to generate in the nitration reaction process.Chlorobenzene thermal insulation nitration product nitro-chlorobenzene mixture mainly contains o-Nitrochlorobenzene, m-nitrochlorobenzene and p-Nitrophenyl chloride, the nitro-chlorobenzene mixture need could satisfy further separation requirement usually after small amount of acid in the oil phase material and the phenolic compound in the material are removed in washing, alkali cleaning, washing, obtaining o-Nitrochlorobenzene, m-nitrochlorobenzene, p-Nitrophenyl chloride product through further separating.The washing impurity-removing technology of traditional thick product of nitro-chlorobenzene adopts a water to carry out mixing, washing, not only produces to contain organic waste water in a large number, but also can cause product losses.
Prepare in the vacuum flashing process of nitro-chlorobenzene in the chlorobenzene nitration reaction, unreacted raw material chlorobenzene volatilizees with water vapor in the material, through producing waste water in the laggard entry phase materials of condensation, mainly contain chlorobenzene and a spot of nitro-chlorobenzene in the waste water that produces in the production process.This waste water generally is difficult to biochemical conversion, and therefore, this waste water is difficult to handle with biochemical process.
Summary of the invention
The purpose of this invention is to provide comprehensive utilization of waste water in a kind of chlorobenzene thermal insulation nitration process and treatment process: adopting the technology of the waste water that produces in the extraction-adsorbing coupled technical finesse chlorobenzene thermal insulation nitration process, is the comprehensive utilization of waste water in a kind of consuming little energy, the safe chlorobenzene thermal insulation nitration feed separation process and the technology and the technology of processing.
The technical scheme that realizes above-mentioned purpose is: the comprehensive utilization and the treatment process of waste water in a kind of chlorobenzene thermal insulation nitration feed separation process is characterized in that described method steps is as follows:
(1) vacuum flashing: in vacuum flashing equipment, the material behind the chlorobenzene thermal insulation nitration is carried out vacuum flashing, the material after the vacuum flashing enters next step;
(2) solution-air is separated: in the solution-air separating device, the material that previous step is obtained carries out the solution-air separation, gaseous phase materials enters next step, the oil phase that liquid phase material obtains through liquid-liquid separation is the thick product of nitro-chlorobenzene, enter the further processing of the 5th step, water is that aqueous sulfuric acid recycles as nitration mixture batching in the chlorobenzene thermal insulation nitration process;
(3) cooling condensation: in the cooling condensing equipment, the gaseous phase materials that previous step is obtained carries out indirect heat exchange cooling condensation, and condensed material enters next step;
(4) liquid-liquid separation: in liquid-liquid separation equipment, the oil phase chlorobenzene that the phlegma of previous step is obtained behind liquid-liquid separation reclaims, and the raw material as nitration reaction uses then, and the water material enters next step;
(5) mixing, washing: in mixing, washing equipment, the thick product of oil phase nitro-chlorobenzene that obtains in water material that previous step is obtained and the solution-air sepn process of second step mixes, blended has also played the effect of washing simultaneously, and the material behind mixing, washing enters next step;
(6) liquid-liquid separation: in liquid-liquid separation equipment, the liquid phase material that previous step is obtained carries out liquid-liquid separation, oil phase is that the thick product of nitro-chlorobenzene goes further to handle and separation and purification, obtains o-Nitrochlorobenzene, m-nitrochlorobenzene and p-Nitrophenyl chloride product, and the water material enters next step;
(7) extraction: in extraction and stripping apparatus, as extraction agent, the processing wastewater that previous step is obtained and other waste water in the chlorobenzene thermal insulation nitration process carry out extraction treatment with chlorobenzene, and the organism in the water material is come together in the extraction phase;
(8) liquid-liquid separation: in liquid-liquid separation equipment, the material that previous step is obtained carries out liquid-liquid separation, and the extraction phase chlorobenzene goes to recycle, and extracting phase waste water enters next step;
(9) absorption: in an adsorption device, the waste water that previous step is passed through extraction treatment further adopts adsorption method to carry out the deep removal organism;
(10) solid-liquid separates: in the solid-liquid separating device, the previous step material is separated the processing that the solid-phase material that obtains removes further to carry out solid waste through solid-liquid, water is that waste water enters the industrial sewage treatment system and further handles.
Further, the mixing, washing equipment described in the 5th step mixing, washing is any one in stirring tank or tube mixer or the static mixer, and the mixing, washing service temperature is 40 ℃-80 ℃.
Further, the liquid-liquid separation equipment described in the 4th step, the 6th step and the 8th step is any one in the centrifugal or efficient water-and-oil separator of decanter type.
Further, extraction equipment described in the 7th step is any one in chamber type extraction apparatus or tower extraction equipment or the static mixing extractor, the extraction agent chlorobenzene that extracting and separating is used and the volume ratio of waste water are 1: 10-1: 100, and the extracting operation temperature is 20 ℃-60 ℃.
Further, an adsorption device in described the 9th step is any one in stirring tank or tube mixer or the static mixer, the adsorption operations temperature is 0 ℃-60 ℃, sorbent material is the mixture of any one or any two kinds or any three kinds of components in flyash or molecular sieve or activated carbon or the diatomite, and the quality of sorbent material and the volume ratio of waste water are 10kg-100kg: 1m
3
Further, the solid-liquid tripping device described in the tenth step is any one in decanter type or filtering type or centrifugal or the vane-type solid-liquid tripping device.
The comprehensive utilization of waste water and the principle of work of treatment process are in the chlorobenzene thermal insulation nitration feed separation process of the present invention: (1) adopts the technology of the waste water that produces in the extraction-adsorbing coupled technical finesse chlorobenzene thermal insulation nitration process; (2) utilize processing wastewater that flash vaporization process produces as flash distillation after the bath water of thick product, can reduce the washing water consumption like this, reclaim the sulfuric acid in the thick product, reduced the loss of product simultaneously; (3) the raw material chlorobenzene of at first producing nitro-chlorobenzene with the chlorobenzene nitration reaction before wastewater treatment enters organic phase as the organism in the extraction agent extraction wastewater, after extracting, can guarantee that organic content is controlled in certain scope in the waste water, and can reclaim the organism in the waste water.
Realize that the main technique equipment that the present invention needs is: mixing, washing equipment (stirring tank, tube mixer or static mixer), extraction equipment, an adsorption device, solid-liquid separating device, liquid-liquid separation equipment etc.
Adopt the advantage of technique scheme to be: (1) with the processing wastewater of by-product in the chlorobenzene nitrifying process as the bath water of nitro-chlorobenzene slightly, can save the bath water amount of process on the one hand, also can reduce wastewater treatment capacity on the other hand, simultaneously can fully recycle chlorobenzene and nitro-chlorobenzene, and provide very favorable condition for thick Separation of Nitrochlorobenzenes is refining, help the cleaner production of implementation procedure, reduced production cost significantly, be convenient to realize large-scale industry enforcement; (2) the raw material chlorobenzene that at first adopts the chlorobenzene nitration reaction to produce nitro-chlorobenzene before waste water treatment process is handled enters organic phase as the organism in the extraction agent extraction wastewater, through guaranteeing that organic content is controlled in certain scope in the waste water after the extraction, and can reclaim organism in the waste water, the extraction phase material that obtains is through recyclable chlorobenzene after the fractionation by distillation, use as reactant feed, the material that can make full use of this production plant area is handled and is fully utilized; (3) waste water behind extracting operation adopts adsorption method further to remove organism; (4) waste water after adsorption treatment satisfies industrial wastewater discharge and requires to enter the industrial sewage treatment system and further handle.Technology of the present invention has that wastewater flow rate is few, by-product recovery utilization and be convenient to the characteristics of industrial implementation.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
The present invention is further detailed explanation below in conjunction with drawings and Examples.
Embodiment one
Main technique equipment is: extraction equipment, an adsorption device and liquid-liquid separation equipment etc.
As shown in Figure 1, the comprehensive utilization and the treatment process of waste water in a kind of chlorobenzene thermal insulation nitration feed separation process is characterized in that described method steps is as follows:
(1) vacuum flashing: the absolute working pressure in flash tank is 0.02MPa, and the material behind the 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 enters next step;
(2) solution-air is separated: in the air-water separator, the material that previous step is obtained carries out the solution-air separation, gaseous phase materials enters next step, the oil phase that liquid phase material obtains through liquid-liquid separation is the thick product of nitro-chlorobenzene, enter the further processing of the 5th step, water is that aqueous sulfuric acid recycles as nitration mixture batching in the chlorobenzene thermal insulation nitration process;
(3) cooling condensation: in plate-type condenser, the gaseous phase materials that previous step is obtained carries out indirect heat exchange cooling condensation, and the temperature out of phlegma is about 20 ℃, and condensed material enters next step;
(4) liquid-liquid separation: in efficient water-and-oil separator, the oil phase chlorobenzene that the phlegma of previous step is obtained behind liquid-liquid separation reclaims, and the raw material as nitration reaction uses then, and the water material enters next step;
(5) mixing, washing: mix in the washing plant in the still formula, the mixing, washing service temperature is 40 ℃, water material that previous step is obtained and the liquid phase material that obtains after second step, solution-air was separated pass through the thick product of oil phase material nitro-chlorobenzene that liquid-liquid separation obtains and carry out mixing, washing, sulfuric acid and the organism carried secretly in the thick product of nitro-chlorobenzene are entered in the water material, and the material behind mixing, washing enters next step;
(6) liquid-liquid separation: in efficient water-and-oil separator, the liquid phase material that previous step is obtained carries out liquid-liquid separation, oil phase is that the thick product of nitro-chlorobenzene goes further to handle and separation and purification, obtains o-Nitrochlorobenzene, m-nitrochlorobenzene and p-Nitrophenyl chloride product, and the water material enters next step;
(7) extraction: in chamber type extraction apparatus (i.e. mixing-clarifying tank), with chlorobenzene as extraction agent, the processing wastewater that previous step is obtained and other waste water in the chlorobenzene thermal insulation nitration process carry out extracting operation, the extraction agent chlorobenzene that extracting and separating is used and the volume ratio of waste water are 1: 10, the extracting operation temperature is 20 ℃, organism in the water material is come together into extraction phase, enter next step then;
(8) liquid-liquid separation: in efficient water-and-oil separator, the material that previous step is obtained carries out liquid-liquid separation, and the extraction phase chlorobenzene goes to recycle, and extracting phase waste water enters next step;
(9) absorption: in the stirring tank an adsorption device, the adsorption operations temperature is 0 ℃, and sorbent material is a flyash, and the quality of adsorbent powder coal ash and the volume ratio of waste water are 100kg: 1m
3, further adopt adsorption method to carry out the deep removal organism waste water of previous step process extraction treatment;
(10) solid-liquid separates: in decanter type solid-liquid tripping device, the previous step material is separated the processing that the solid-phase material that obtains removes further to carry out solid waste through solid-liquid, water is that waste water enters the industrial sewage treatment system and further handles.
Embodiment two
Main technique equipment is: extraction equipment, an adsorption device and liquid-liquid separation equipment etc.
As shown in Figure 1, the comprehensive utilization and the treatment process of waste water in a kind of chlorobenzene thermal insulation nitration feed separation process is characterized in that described method steps is as follows:
(1) vacuum flashing: in flash cooler, at absolute working pressure is 0.04MPa, material behind the 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 enters next step;
(2) solution-air is separated: in liquid-gas separator, the material that previous step is obtained carries out the solution-air separation, gaseous phase materials enters next step, the oil phase that liquid phase material obtains through liquid-liquid separation is the thick product of nitro-chlorobenzene, enter the further processing of the 5th step, water is that aqueous sulfuric acid recycles as nitration mixture batching in the chlorobenzene thermal insulation nitration process;
(3) cooling condensation: in shell-and tube condenser, the gaseous phase materials that previous step is obtained carries out indirect heat exchange cooling condensation, and the temperature out of phlegma is about 40 ℃, and the condensed material of cooling condensing equipment enters next step;
(4) liquid-liquid separation: in centrifugal liquid liquid separator, the oil phase chlorobenzene that the phlegma of previous step is obtained behind liquid-liquid separation reclaims, and the raw material as nitration reaction uses then, and the water material enters next step;
(5) mixing, washing: in tubular type mixing, washing device, the mixing, washing service temperature is 60 ℃, water material that previous step is obtained and the liquid phase material that obtains after second step, solution-air was separated pass through the thick product of oil phase material nitro-chlorobenzene that liquid-liquid separation obtains and carry out mixing, washing, sulfuric acid and the organism carried secretly in the thick product of nitro-chlorobenzene are entered in the water material, and the material behind mixing, washing enters next step;
(6) liquid-liquid separation: in centrifugal liquid liquid separator, the liquid phase material that previous step is obtained carries out liquid-liquid separation, oil phase is that the thick product of nitro-chlorobenzene goes further to handle and separation and purification, obtains o-Nitrochlorobenzene, m-nitrochlorobenzene and p-Nitrophenyl chloride product, and the water material enters next step;
(7) extraction: in sieve-tray tower, with chlorobenzene as extraction agent, the processing wastewater that previous step is obtained and other waste water in the chlorobenzene thermal insulation nitration process carry out extracting operation, the extraction agent chlorobenzene that extracting and separating is used and the volume ratio of waste water are 1: 50, the extracting operation temperature is 40 ℃, organism in the water material is come together into extraction phase, enter next step then;
(8) liquid-liquid separation: in centrifugal liquid liquid separator, the material that previous step is obtained carries out liquid-liquid separation, and the extraction phase chlorobenzene goes to recycle, and extracting phase waste water enters next step;
(9) adsorbing and removing organism: in the tubular type an adsorption device, the adsorption operations temperature is 20 ℃, is that 70%: 30% the flyash and the mixture of two kinds of components of diatomite are sorbent material with mass ratio, and the quality of sorbent material and the volume ratio of waste water are 50kg: 1m
3, further adopt adsorption method to carry out the deep removal organism waste water of previous step process extraction treatment;
(10) solid-liquid separates: in centrifugal solid-liquid tripping device, the previous step material is separated the processing that the solid-phase material that obtains removes further to carry out solid waste through solid-liquid, water is that waste water enters the industrial sewage treatment system and further handles.
Embodiment three
Main technique equipment is: extraction equipment, an adsorption device and liquid-liquid separation equipment etc.
As shown in Figure 1, the comprehensive utilization and the treatment process of waste water in a kind of chlorobenzene thermal insulation nitration feed separation process is characterized in that described method steps is as follows:
(1) vacuum flashing: in flashing tower, absolute working pressure in flashing tower is 0.08MPa, material behind the 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 enters next step;
(2) solution-air is separated: in the Sofitel air water separator, the material that previous step is obtained carries out the solution-air separation, gaseous phase materials enters next step, the oil phase that liquid phase material obtains through liquid-liquid separation is the thick product of nitro-chlorobenzene, enter the further processing of the 5th step, water is that aqueous sulfuric acid recycles as nitration mixture batching in the chlorobenzene thermal insulation nitration process;
(3) cooling condensation: in shell and-tube condenser, the gaseous phase materials that previous step is obtained carries out indirect heat exchange cooling condensation, and the temperature out of phlegma is about 60 ℃, and condensed material enters next step;
(4) liquid-liquid separation: in the decanter type liquid liquid separator, the oil phase chlorobenzene that the phlegma of previous step is obtained behind liquid-liquid separation reclaims, and the raw material as nitration reaction uses then, and the water material enters next step;
(5) mixing, washing: in the static mixing washer, the mixing, washing service temperature is 80 ℃, water material that previous step is obtained and the liquid phase material that obtains after second step, solution-air was separated pass through the thick product of oil phase material nitro-chlorobenzene that liquid-liquid separation obtains and carry out mixing, washing, sulfuric acid and the organism carried secretly in the thick product of nitro-chlorobenzene are entered in the water material, and the material behind mixing, washing enters next step;
(6) liquid-liquid separation: in the decanter type liquid liquid separator, the liquid phase material that previous step is obtained carries out liquid-liquid separation, oil phase is that the thick product of nitro-chlorobenzene goes further to handle and separation and purification, obtains o-Nitrochlorobenzene, m-nitrochlorobenzene and p-Nitrophenyl chloride product, and the water material enters next step;
(7) extraction: in the static mixing extractor, with chlorobenzene as extraction agent, the processing wastewater that previous step is obtained and other waste water in the chlorobenzene thermal insulation nitration process carry out extracting operation, the extraction agent chlorobenzene that extracting and separating is used and the volume ratio of waste water are 1: 100, the extracting operation temperature is 60 ℃, organism in the water material is come together into extraction phase, enter next step then;
(8) liquid-liquid separation: in the decanter type liquid liquid separator, the material that previous step is obtained carries out liquid-liquid separation, and the extraction phase chlorobenzene goes to recycle, and extracting phase waste water enters next step;
(9) adsorbing and removing organism: in the static mixer an adsorption device, the adsorption operations temperature is 60 ℃, is that 50%: 50% the flyash and the mixture of two kinds of components of gac are sorbent material with mass ratio, and the quality of sorbent material and the volume ratio of waste water are 10kg: 1m
3, further adopt adsorption method to carry out the deep removal organism waste water of previous step process extraction treatment;
(10) solid-liquid separates: in vane-type solid-liquid tripping device, the previous step material is separated the processing that the solid-phase material that obtains removes further to carry out solid waste through solid-liquid, water is that waste water enters the industrial sewage treatment system and further handles.
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 (6)
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| 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 |
| CN101851041B (en) * | 2010-04-27 | 2012-02-08 | 中国海诚工程科技股份有限公司 | Method and device for realizing zero release in desulfuration wastewater deepening treatment |
| CN103073139A (en) * | 2011-10-26 | 2013-05-01 | 中国石油化工股份有限公司 | Method and device used for processing nitrochlorobenzene production wastewater |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1209419A (en) * | 1997-08-21 | 1999-03-03 | 武汉大学 | Noval method for treatment of nitro-waste-water |
| CN1371902A (en) * | 2001-02-23 | 2002-10-02 | 拜尔公司 | Continuous thermo-insulation method for production of nitro-chlorobenzene |
| DE102006013579B3 (en) * | 2006-03-22 | 2007-08-23 | Plinke Gmbh | Reducing the waste water quantity during dinitrotoluene production, and optimizing the waste water quality comprises stripping the waste acid and pre-purified waste acid, saturating the sulfuric acid and purifying the nitrous gases |
-
2009
- 2009-07-07 CN CN2009101822892A patent/CN101602561B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1209419A (en) * | 1997-08-21 | 1999-03-03 | 武汉大学 | Noval method for treatment of nitro-waste-water |
| CN1371902A (en) * | 2001-02-23 | 2002-10-02 | 拜尔公司 | Continuous thermo-insulation method for production of nitro-chlorobenzene |
| DE102006013579B3 (en) * | 2006-03-22 | 2007-08-23 | Plinke Gmbh | Reducing the waste water quantity during dinitrotoluene production, and optimizing the waste water quality comprises stripping the waste acid and pre-purified waste acid, saturating the sulfuric acid and purifying the nitrous gases |
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| CN101602561A (en) | 2009-12-16 |
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