CN1067980C - Method for extracting nitrochlorbenzene from wastes of producing p-/o-nitrochlorbenzene - Google Patents
Method for extracting nitrochlorbenzene from wastes of producing p-/o-nitrochlorbenzene Download PDFInfo
- Publication number
- CN1067980C CN1067980C CN96116979A CN96116979A CN1067980C CN 1067980 C CN1067980 C CN 1067980C CN 96116979 A CN96116979 A CN 96116979A CN 96116979 A CN96116979 A CN 96116979A CN 1067980 C CN1067980 C CN 1067980C
- Authority
- CN
- China
- Prior art keywords
- nitrochlorobenzene
- tower
- rectifying
- crystallization
- lightness
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention discloses a method for extracting nitrochlorobenzene from the waste material from the production of p-nitrochlorobenzene and o-nitrochlorobenzene. On the basis of the prior art, a light impurity removing treatment is carried out for removing the light impurities of chlorobenzene, dichloro-benzene, nitrobenzene, etc., and useful constituents can be extracted from the waste material in multiple cycles. With the utilization of the present invention, not only the p-nitrochlorobenzene and the o-nitrochlorobenzene, but also m-nitrochlorobenzene can be extracted, and simultaneously, the total yield of products is greatly improved (the total yield reaches 95%); in addition, compared with the prior art, the present invention has the advantages of low material cost, low equipment investment, short period, high yield, little pollution, etc.
Description
The present invention relates to a kind of method of from produce waste material, further extracting, adjacent, m-nitrochlorobenzene to, o-Nitrochlorobenzene.
The production of domestic m-nitrochlorobenzene all is raw material with oil of mirbane, chlorination in the chlorination tower then, wash again, neutralization, rectifying, crystallization form; This production method facility investment is big, complex process, the cycle is long, cost is high; At present, domestic also have the production of utilization right, it is right that the waste material of o-Nitrochlorobenzene extracts through rectifying again, o-Nitrochlorobenzene, but, they just go out trash discharge after only finishing and once extracting, can't utilize again, in fact, at this moment only extracted 50% of the useful component that contains in the waste material, 50% useful component still is present in the waste material of secondary emission in addition, owing to contain 3% chlorobenzene approximately in the waste material, impurity such as dichlorobenzene and oil of mirbane, these impurity are not removed, can't extract m-nitrochlorobenzene, also just can't further extract surplus have right in the waste material, o-Nitrochlorobenzene causes serious waste, and the discharging of waste material simultaneously pollutes environment; Existing in addition production technology can't be utilized the waste material that contains m-nitrochlorobenzene 〉=30%.
The object of the present invention is to provide a kind of method of from produce waste material, extracting nitro-chlorobenzene, use this method not only can from waste material, extract m-nitrochlorobenzene, improved yield simultaneously greatly, o-Nitrochlorobenzene to, o-Nitrochlorobenzene.
The objective of the invention is to be achieved through the following technical solutions: at first with waste material through rectifying one tower rectifying, separate, crystallization goes out p-Nitrophenyl chloride and o-Nitrochlorobenzene, the low oil of the crystallization of o-Nitrochlorobenzene returns rectifying one tower, the low oil of the crystallization of p-Nitrophenyl chloride is sent into lightness-removing column, when lightness-removing column tower bottoms position 〉=1/2, slowly sending into 0.6-1.0MPa steam in lightness-removing column heats, 140-160 ℃ of control tower temperature in the kettle, simultaneously send cold water to overhead condenser, 40-50 ℃ of control leaving water temperature(LWT), when tower top temperature reaches 90-110 ℃, total reflux operation 0.5-1.0 hour, zero pour and stratographic analysis are surveyed in sampling, when zero pour≤7 ℃, a position, contraposition nitro-chlorobenzene＜10% o'clock, the extraction chlorobenzene, enter rectifying two towers behind dichlorobenzene and the oil of mirbane, rectifying, separate, crystallization goes out m-nitrochlorobenzene and p-Nitrophenyl chloride, the low oily recirculation of the crystallization of m-nitrochlorobenzene is sent into lightness-removing column and is entered rectifying two tower rectifying through taking off after light, and ortho position content 〉=10% o'clock in the low oil of the crystallization of p-Nitrophenyl chloride enters rectifying one tower; Ortho position content＜10% o'clock in the low oil of crystallization enters rectifying two towers.
The present invention with produce waste material to, o-Nitrochlorobenzene be raw material further repeatedly circulation extract its inner residual nitro-chlorobenzene, because the present invention has taked to take off light processing, impurity such as chlorobenzene, dichlorobenzene and oil of mirbane have been sloughed, thereby can from secondary slugs, extract m-nitrochlorobenzene, extract that the secondary slugs of m-nitrochlorobenzene is capable of circulation carries out multiple extraction as raw material; The present invention not only can extract the ortho para nitro-chlorobenzene, but also can extract m-nitrochlorobenzene, and total yield of products improves (total recovery reaches 95%, and the prior art yield is 50%) greatly simultaneously.
In sum, the present invention has compared with prior art that raw materials cost is low, facility investment is few, the cycle is short and the yield advantages of higher; This technical process does not produce waste water, waste gas in addition, has only a small amount of waste residue, and environmental pollution is little.
Below the invention will be further described:
At first will vacuumize in the tower, vacuum tightness 〉=0.098MPa, startup waste material pump injects waste material with the flow velocity of 200l/h in rectifying one tower, when the liquid level of a Tata still reaches 1/2, slowly send the steam of 1.2-1.3MPa to heat to a tower reboiler, the control tower temperature is sent water coolant to tower item condenser simultaneously at 150-160 ℃, about 80 ℃ of control leaving water temperature(LWT)s, when tower top temperature reaches 115-130 ℃, total reflux operation 0.5-1.0 hour, look a tower level condition, reduce or suspend charging; Getting cat head sample survey zero pour is 45-55 ℃, when ortho position content in the fraction＜5%, the extraction of cat head fraction, dominant discharge 100-110l/h adopts into rich contraposition cylinder, after the one cat head fraction extraction, advance waste material according to a Tata still level condition, control inlet amount 160-180l/h, carry out stable operation, get the cat head sample in per 2 hours and survey zero pour, do stratographic analysis, when zero pour 〉=22 ℃, ortho position content 〉=85% o'clock, open a tower extraction valve with the 70l/h flow velocity to decoking one tower extraction one tower fraction, when decoking one tower liquid level reaches 3/4, slowly in this tower, send into the steam heating of 1.0MPa, 140-160 ℃ of control tower still temperature, simultaneously send water coolant to the decoking overhead condenser, 40-50 ℃ of control leaving water temperature(LWT), tower top temperature is in the time of 120-130 ℃, after the total reflux 0.5 hour, carry out the extraction of cat head fraction, adopt into rich ortho position cylinder, when rich contraposition cylinder liquid level 〉=3/4, this material squeezed into the nitre crystallizer is carried out crystallization, the low oil of crystallization is put into the lightness-removing column still, when lightness-removing column still liquid level 〉=1/2, slowly steam from 0.8MPa to the lightness-removing column still that send into heats, about 140 ℃ of control tower still temperature, simultaneously send water coolant to this column overhead condenser, 40 ℃ of control leaving water temperature(LWT)s, when the lightness-removing column tower top temperature reaches 90 ℃, total reflux 0.5 hour, zero pour and stratographic analysis are surveyed in sampling, when zero pour≤7 ℃, between, contraposition content＜10% o'clock, with chlorobenzene, light component extraction such as dichlorobenzene and oil of mirbane, adopt into light component storage tank, when light component content in the material in the lightness-removing column still≤2% when (the about 30-40 of zero pour ℃), material is squeezed into rectifying two towers with the flow velocity of 200l/h, rectifying two tower liquid level 〉=1/2 o'clock, slowly the steam that reboiler is sent into 1.2-1.3MPa in it heats, 150-165 ℃ of control tower still temperature, when tower top temperature reaches 115-130 ℃, carried out total reflux 1-2 hour, look tower bottoms position situation, reduce or stop charging, get the cat head sample and survey zero pour and stratographic analysis, when zero pour through 30-40 ℃, contraposition content≤15% o'clock, the extraction of cat head fraction, adopt position cylinder between richness with flow velocity 30-40l/h, look tower bottoms position situation simultaneously, give rectifying two tower chargings with the 90-130l/h flow velocity, after two column overhead fraction extraction a few hours of rectifying, get two Tata still samples and survey zero pour and stratographic analysis, when zero pour 〉=50 ℃, between position content≤35% o'clock, flow velocity with 60-90l/h is squeezed into decoking two towers to two tower materials, when decoking two tower liquid levels 〉=1/2, slowly feeds the 0.9-1.0MPa steam heating, 150-160 ℃ of control tower still temperature, simultaneously send water coolant to this column overhead condenser, about 70 ℃ of control leaving water temperature(LWT)s are when the tower top temperature of decoking two towers reaches 120-130 ℃, after the total reflux 0.5 hour, fraction is adopted into rich contraposition cylinder with the flow velocity of 60-90l/h; When this rich contraposition cylinder liquid level 〉=1/2, to squeeze into the nitre crystallizer is carried out the nitre crystallization, the low oil of this crystallization is sent into rectifying one tower and is used; When rich ortho position cylinder liquid level 〉=3/4, to squeeze into adjacent nitre crystallizer and carry out adjacent nitre crystallization, the low oil of adjacent nitre crystallization is sent into rectifying one tower and is used; When position cylinder liquid level between richness 〉=1/2, to squeeze into a nitre crystallizer and carry out a nitre crystallization, the low oil of a nitre crystallization is put into the lightness-removing column still and is taken off light laggard rectifying two towers.
Embodiment two: in taking off the light industry preface, when lightness-removing column still liquid level 〉=1/2, slowly steam from 0.6MPa to the lightness-removing column still that send into heats, about 150 ℃ of control tower still temperature, simultaneously send water coolant to this column overhead condenser, 45 ℃ of control leaving water temperature(LWT)s, when the lightness-removing column tower top temperature reaches 100 ℃, total reflux 1.0 hours, zero pour and stratographic analysis are surveyed in sampling, when zero pour≤7 ℃,, contraposition content＜10% o'clock, with light component extraction such as chlorobenzene, dichlorobenzene and oil of mirbane, other process operations are identical with embodiment one.
Embodiment three: in taking off the light industry preface, when lightness-removing column still liquid level 〉=1/2, slowly steam from 1.0MPa to the lightness-removing column still that send into heats, about 160 ℃ of control tower still temperature, simultaneously send water coolant to this column overhead condenser, 50 ℃ of control leaving water temperature(LWT)s, when the lightness-removing column tower top temperature reaches 110 ℃, total reflux 0.5 hour, zero pour and stratographic analysis are surveyed in sampling, when zero pour≤7 ℃,, contraposition content＜10% o'clock, with light component extraction such as chlorobenzene, dichlorobenzene and oil of mirbane, other process operations are identical with embodiment one.
In addition, whole distillation operation will keep that vacuum is stable, the tower bottoms position stable and heating steam is pressed stable.
Claims (1)
1, right from producing, extract the method for nitro-chlorobenzene in the waste material of o-Nitrochlorobenzene, at first with waste material through rectifying one tower rectifying, separate, crystallization goes out p-Nitrophenyl chloride and o-Nitrochlorobenzene, the low oil of the crystallization of o-Nitrochlorobenzene returns rectifying one tower, it is characterized in that: the low oil of the crystallization of p-Nitrophenyl chloride is sent into lightness-removing column, when lightness-removing column tower bottoms position 〉=1/2, slowly sending into 0.6-1.0MPa steam in lightness-removing column heats, 140-160 ℃ of control tower temperature in the kettle, simultaneously send cold water to overhead condenser, 40-50 ℃ of control leaving water temperature(LWT), when tower top temperature reaches 90-110 ℃, total reflux operation 0.5-1.0 hour, zero pour and stratographic analysis are surveyed in sampling, when zero pour≤7 ℃, between the position, contraposition nitro-chlorobenzene＜10% o'clock, the extraction chlorobenzene, enter rectifying two towers behind dichlorobenzene and the oil of mirbane, rectifying, separate, crystallization goes out m-nitrochlorobenzene and p-Nitrophenyl chloride, the low oily recirculation of the crystallization of m-nitrochlorobenzene is sent into lightness-removing column and enter rectifying two tower rectifying after being taken off gently, ortho position content 〉=10% o'clock in the low oil of the crystallization of p-Nitrophenyl chloride enters rectifying one tower; Ortho position content＜10% o'clock in the low oil of crystallization enters rectifying two towers.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96116979A CN1067980C (en) | 1996-06-22 | 1996-06-22 | Method for extracting nitrochlorbenzene from wastes of producing p-/o-nitrochlorbenzene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96116979A CN1067980C (en) | 1996-06-22 | 1996-06-22 | Method for extracting nitrochlorbenzene from wastes of producing p-/o-nitrochlorbenzene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1169984A CN1169984A (en) | 1998-01-14 |
| CN1067980C true CN1067980C (en) | 2001-07-04 |
Family
ID=5123925
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96116979A Expired - Fee Related CN1067980C (en) | 1996-06-22 | 1996-06-22 | Method for extracting nitrochlorbenzene from wastes of producing p-/o-nitrochlorbenzene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1067980C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111689865A (en) * | 2019-03-15 | 2020-09-22 | 中石化南京化工研究院有限公司 | Method for extracting effective components from o-nitrochlorobenzene tar |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5163210A (en) * | 1974-11-20 | 1976-06-01 | Marui Kako Kk | Nogyoyohashuhoho oyobisono sochi |
| JPS632956A (en) * | 1986-06-20 | 1988-01-07 | Hodogaya Chem Co Ltd | Method for separating dichloronitrobenzene isomers |
-
1996
- 1996-06-22 CN CN96116979A patent/CN1067980C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5163210A (en) * | 1974-11-20 | 1976-06-01 | Marui Kako Kk | Nogyoyohashuhoho oyobisono sochi |
| JPS632956A (en) * | 1986-06-20 | 1988-01-07 | Hodogaya Chem Co Ltd | Method for separating dichloronitrobenzene isomers |
Non-Patent Citations (1)
| Title |
|---|
| 河北化工1992年第1期 1992.1.1 顾伯琴等对，邻硝基氯苯生产中下脚低油的综合利用 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1169984A (en) | 1998-01-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104817481B (en) | Technological method for recovering DMSO from DMSO aqueous solution | |
| CN105967425A (en) | Coal chemical industry grey water flashing treatment system capable of reducing ammonia accumulation and coal chemical industry grey water flashing treatment process capable of reducing ammonia accumulation | |
| CN107903149A (en) | A kind of coproduction absolute ethyl alcohol, the devices and methods therefor of electronic grade anhydrous ethanol | |
| CN101735045A (en) | Method for producing ethyl acetate by using entrainer | |
| CN101266102A (en) | Cane sugar factory waste water zero discharge process | |
| CN108546243A (en) | A kind of lithium battery production double tower NMP recycling purification systems and its recycling method of purification | |
| CN101088975A (en) | Fuel alcohol dewatering apparatus and process | |
| CN1067980C (en) | Method for extracting nitrochlorbenzene from wastes of producing p-/o-nitrochlorbenzene | |
| CN106831472A (en) | A kind of DMF salt bearing liquid wastes recovery process and system | |
| CN214327607U (en) | Tetrahydrofuran recycling and refining device | |
| CN103274568A (en) | Method for treating ketone-containing wastewater in cyclohexanone ammoximation device by employing extraction method | |
| CN110668910B (en) | Benzene distillation residue recovery device, recovery method and application | |
| CN210367856U (en) | Device for continuously treating waste metal sodium | |
| CN202181270U (en) | Device for rectifying and purifying m-nitrotoluene coarse products | |
| CN206896878U (en) | A kind of device for being dehydrated ternary azeotrope by extracting rectifying | |
| CN111333480A (en) | Butadiene refining method and device | |
| CN108854456B (en) | System and method for recycling heat energy of desorption tower | |
| CN210419808U (en) | Fusel recovery system in BDO device waste liquid | |
| CN201214026Y (en) | Tail-gas recovery device | |
| CN104610173B (en) | A kind of cycle production process of nigrosine | |
| CN103588734B (en) | Recovery method and recovery device of butyl ester and acetone in ketene dimer production | |
| CN209934112U (en) | Continuous separation and recovery device for organic solvent waste liquid | |
| CN204569785U (en) | A kind of device reclaiming DMSO from the DMSO aqueous solution | |
| CN208949058U (en) | A kind of coal gasification phenol wastewater ammonia still process extraction multiple treating system | |
| CN203295403U (en) | Device system used for extracting and refining azophenylene in RT base waste |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |