CN101704726A - Continuous refinement separation device and method of coked crude phenol - Google Patents
Continuous refinement separation device and method of coked crude phenol Download PDFInfo
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Abstract
The invention relates to a continuous refinement separation device and method of coked crude phenol. The continuous refinement separation device comprises a static mixer 1, a first stage pretreatment acid-adding unit composed of a first stage mixing slot 2 and a wipe film evaporator 3, a second stage pretreatment oxidation unit composed of a second stage mixing slot 4 and a buffer tank, a phenol residue removing tower 6 and a rectification tower system composed of a dewatering tower 7, a phenol refinement tower 8, a orthocresol refinement tower 9 and a m,p-cresol refinement tower 10, wherein the first stage pretreatment acid-adding unit is connected with the phenol residue removing tower, the phenol residue removing tower is connected with the second stage pretreatment oxidation unit, and then all devices of the refinement tower system are connected together in turn. The device and method of the invention can effectively performs processes of decoloring, deodorizing, desulfurizing, removing impurity and the like to the coked crude phenol raw material through reasonable design to obtain more than 99.5wt% of high purity phenol, more than 99.0wt% of high purity orthocresol, more than 99.0wt% of high purity m,p-cresol and xylenol product. The whole process is reasonable, has high degree of automation and is characterized by low process energy consumption, high product quality, good stability and the like, thus the method of the invention is an effective and feasible coked crude phenol continuous refinement separation technology.
Description
Technical field
The invention belongs to the device and method of chemical separation process, relate to a kind of process for purification of coking crude phenols, is exactly the continuous rectification tripping device and the method for coking crude phenols specifically.
Background technology
The coking phenols is one of main Chemicals of extracting in the coal tar, the composition of each crude phenols raw material is relevant with the condition of coal blending composition, coal blending character and coal tar operation thereof with productive rate, its source comes from the carbolic oil cut that produces in the coal tar fractional distillation on the one hand, come from the phenolic compound from the phenolic wastewater extraction that produces from coal gasification course on the other hand, the crude phenols component in two sources all contains impurity such as phenol, ortho-cresol, M-and P-cresols, water, xylenol, higher phenols and pitch thereof basically.
Phenol products such as phenol, ortho-cresol, M-and P-cresols and xylenol cut all are important chemical material, wherein phenol is mainly used to produce resol, Resins, epoxy, ion exchange resin, synthon and as sanitas and sterilizing agent, its application is very extensive; Ortho-cresol, M-and P-cresols then have stronger sterilizing ability and toxicity bigger, can be used as the sanitas of timber, railroad tie and the sterilizing agent in the medical treatment thereof; The xylenol cut is the mixture of six kinds of isomerss, and mainly as synthetic resins, insullac etc., its application is also very extensive.Phenolic compound is important organic synthesis raw material, development along with chemical industry, the discharging contain phenol and amphyl waste water in continuous increase, the toxicity of phenolic wastewater can have a strong impact on the eubiosis of water resources, therefore handles, reclaims and utilize phenolic wastewater and carbolic oil component thereof to become an important research work.
Reclaim crude phenols and used the history in more than 100 year from coal tar phenol water, the various countries investigator has all invented multiple recovery and has handled the technology of crude phenols.No matter be crude phenols cut in the coal tar and the crude phenols that reclaim from coking chemical waste water,, before carrying out rectifying, it all needs raw material carried out pretreatment operation such as deodorization, desulfurization and decolouring if obtain highly purified phenol products.About the fine purification treatment process of phenolic compound, most treating processes that all relate to chemosynthesis phenol seldom relate to the processing of coking crude phenols at present.Wherein Chinese patent CN1279231A discloses a kind of process for purification of coarse phenol containing sulfur, add NaOH or KOH solution exactly and hydrogen peroxide alkalizes and oxide treatment, but this technology mainly is the technology at crude phenols exploitation in the oil lightweight oil, then there are shortcomings such as long processing period, decolouring and deodorising effect be relatively poor for the more complicated coking crude phenols of process element, obviously are not suitable for handling the pre-treatment of coking crude phenols.
Japanese Patent JP62-12731 adopts hydrogen peroxide and clay-treated method to come the pre-treatment crude phenols, the compounds such as mercaptan of raw material can be converted into the less disulphide of stink and obtain refining crude phenols by clay-treated method then, experiment shows, this pretreated deodorization and sweetening effectiveness are better, but the poor effect of its decolouring, and the quality product rather unstable behind refining crude phenols is having a strong impact on the refining effect and the recovery value of coking crude phenols.
Because it is less that the raw material total amount of phenols cut accounts for the ratio of coal tar, common 1,000,000 tons/year coal chemical enterprise only produces the crude phenols raw material of about 1-1.2%, and domestic early stage coal chemical enterprise is the scale below 1,000,000 tons/year, the raw material total amount of its crude phenols is less relatively and basically all below 10,000 tons/year, therefore relevant enterprise all adopts equipment simple both at home and abroad, invest less intermittent type rectification under vacuum technology, adopt two towers or three tower batch fractionating tower apparatus and technology to finish exactly and take off slag, dehydration, plurality of processes such as the refining and cresols of phenol is refining, thereby realize reclaiming products such as phenol and cresols. well-known, because the process characteristic of batch fractionating and the sensitive characteristic of phenolic compound thereof, make that certainly existing phenolic compound in the batch fractionating separating technology decomposes, thereby phenomenons such as knot carbon influence the quality and the yield of product, so that the less stable of the quality product of whole technology, simultaneously in the batch fractionating treating processes between its each component interim fraction needs on the high side repeat rectifying and also cause the energy consumption of whole sepn process bigger, obviously from reliability of technology and economy, refining device and the technology thereof of separating crude phenols of batch fractionating has been not suitable for handling on a large scale the coking crude phenols.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art, provide the coking crude phenols continuous industry of a kind of level of automation height, good product quality and good stability to divide from device; Use this device that products such as high-purity phenol, ortho-cresol and M-and P-cresols can be provided.
The continuous rectification tripping device of coking crude phenols of the present invention comprises that the one-level pre-treatment that static mixer 1, one-level steel basin 2 and luwa evaporator 3 are formed adds acid unit; Comprise the secondary pre-treatment oxidation unit that secondary steel basin 4 and surge tank 5 are formed; Dephenolize slag tower 6 and the essence slide Tower System that comprises dehydration tower 7, phenol refining 8 towers, ortho-cresol treating tower 9 and M-and P-cresols treating tower 10; The one-level pre-treatment adds acid unit and connects dephenolize slag tower, and dephenolize slag tower connects secondary pre-treatment oxidation unit, and secondary pre-treatment oxidation unit connects the rectifying tower system.
Crude phenols raw material and concentrated acid solution pipeline are connected to import one end that enters static mixer 1, the outlet of the static mixer the other end is connected to the inlet line on one-level steel basin 2 tops, and the discharging pipeline of bottom directly is connected with the liquid phase feeding mouth on luwa evaporator 3 tops; The upper, middle and lower portion of luwa evaporator 3 is provided with liquid phase feeding mouth, gas phase discharge port and acid sludge row mouth respectively, and the gas phase discharge port on top is connected to the feeding line at dephenolize slag tower 6 middle parts; Dephenolize slag tower 6 cat head discharging pipelines and oxidant feed pipeline all are connected to the feeding line on secondary steel basin 4 tops, the discharging pipeline of secondary steel basin bottom is connected to the opening for feed of surge tank 5 one ends, the surge tank bottom is provided with the acid sludge relief outlet, and the top discharging pipeline of the surge tank the other end is connected with the middle part feeding line of dehydration tower 7; The dehydration tower top connects the vent line of waste water, and the discharging pipeline of bottom is connected with the feeding line at phenol treating tower 8 middle parts; The phenol tower cat head connects the discharging pipeline of phenol product, and the discharging pipeline of tower bottom is connected to the middle part feeding line of ortho-cresol tower 9; The discharging pipeline of the adjoining cresols product of ortho-cresol column overhead, the bottom discharge pipeline is connected with the intermediate feed pipeline of M-and P-cresols tower 10; The p-cresol column overhead connects the discharging pipeline of M-and P-cresols product, and the bottom connects the discharging pipeline of xylenol residue.
The working method of the tripping device of a kind of coking crude phenols of the present invention continuous rectification, step is as follows:
1) crude phenols raw material and concentrated acid solution enter static mixer 1, and then enter one-level steel basin 2 and carry out entering luwa evaporator 3 after thorough mixing stirs, luwa evaporator 3 adopts external jacket formula steam heating, and heavy constituent are discharged in the bottom, and the gaseous component on top enters dephenolize slag tower 6;
2) crude phenols that enter dephenolize slag tower 6 after treatment, discharge heavy constituent at the bottom of the tower, cat head distilled crude phenols and oxygenant enter secondary steel basin 4 to carry out entering surge tank 5 then after mixed oxidization handles, acid sludge is discharged in the surge tank bottom, and the cut that discharge at the top enters dehydration tower 7;
3) dehydration tower 7 tops distillate the waste water that contains a small amount of phenol, and the cut of discharging at the bottom of the tower is to phenol treating tower 8; Phenol product is from 8 extraction of phenol treating tower, and the cut that discharge phenol treating tower bottom is to ortho-cresol treating tower 9;
4) the ortho-cresol product is from the 9 cat head extraction of ortho-cresol treating tower, and the cut that discharge the bottom is to M-and P-cresols treating tower 10;
5) with extraction, the xylenol cut is discharged in the bottom to the M-and P-cresols product from M-and P-cresols treating tower 10.
Described concentrated acid is the sulphuric acid soln of 40.0～60.0wt%, and add-on is 3.0～5.0% of a crude phenols material quantity.Described oxygenant is hydrogen peroxide or ozone, and add-on is 1.0～3.0% of a crude phenols amount.
Continuous rectification separating technology of the present invention adds acid unit, dephenolize slag tower, secondary pre-treatment oxidation unit, dehydration tower, phenol treating tower, ortho-cresol tower and M-and P-cresols tower by the one-level pre-treatment and finishes.
The continuous rectification separating technology of the present invention for forming by five rectifying tower, wherein dephenolize slag Tata internals are the valve tray structure, all the other four Tata internals are high efficiency structured packing tower.
An advantage of the present invention is exactly to consider the physicochemical property of coking crude phenols raw material system, the device of whole separating technology is chosen to be stainless steel, as 304 materials.Thereby the problem of material corrosion resistance nature in the separating technology of having solved has fully guaranteed the quality and the stability of product.
Another advantage of the present invention is exactly to be added acid unit and efficiently solved decolouring, desulfurization, the deodorization of crude phenols raw material jointly and taken off problems such as impurity by the secondary pre-treatment oxide treatment unit that secondary steel basin, surge tank are formed by the one-level pre-treatment that static mixer, one-level steel basin, luwa evaporator are formed, and makes that follow-up purified quality product is very high.
The reboiler that another advantage of the present invention is exactly each rectifying tower is all selected thermosyphon reboiler for use, efficiently solve scenes such as phenolic material quick easy decomposition hot in nature, knot carbon, and this rectifying separation automation technolo degree height, process energy consumption are less, for the large-scale continuous production application of coking crude phenols provides certain advantage, and have favorable economic benefit and social benefit.
The present invention passes through appropriate design, effectively to coking crude phenols raw material decolour, processes such as deodorization, desulfurization and the removal of impurity, can obtain high purity phenol (＞99.5wt%), high-purity o-phenyl phenol (＞99.0wt%), high-purity Pyrogentisinic Acid (＞99.0wt%) and the xylenol product.Whole process flow is reasonable, level of automation is high and have that the process energy consumption is lower, quality product is high and characteristics such as good stability, is a kind of efficient feasible coking crude phenols continuous rectification separating technology.
Description of drawings
Accompanying drawing is a kind of coking crude phenols continuous rectification separation processes schema.
Embodiment
Device and embodiment below in conjunction with accompanying drawing are further elaborated the present invention, but the present invention are not produced any restriction.
Install as shown in drawings: the one-level pre-treatment of being made up of static mixer 1, one-level steel basin 2 and luwa evaporator 3 adds acid unit; The secondary pre-treatment oxidation unit of forming by secondary steel basin 4 and surge tank 5; Also comprise dephenolize slag tower 6 and the rectifying tower system made from extra care 8 towers, ortho-cresol treating tower 9 and M-and P-cresols treating tower 10 by dehydration tower 7, phenol; The one-level pre-treatment adds acid unit and connects dephenolize slag tower, and dephenolize slag tower connects secondary pre-treatment oxidation unit, and secondary pre-treatment oxidation unit connects the rectifying tower system.
Crude phenols raw material and concentrated acid solution pipeline are connected to import one end that enters static mixer 1, the outlet of the static mixer the other end is connected to the inlet line on one-level steel basin 2 tops, and the discharging pipeline of bottom directly is connected with the liquid phase feeding mouth on luwa evaporator 3 tops; The upper, middle and lower portion of luwa evaporator 3 is provided with liquid phase feeding mouth, gas phase discharge port and acid sludge row mouth respectively, and the gas phase discharge port on top is connected to the feeding line at dephenolize slag tower 6 middle parts; Dephenolize slag tower 6 cat head discharging pipelines and oxidant feed pipeline all are connected to the feeding line on secondary steel basin 4 tops, the discharging pipeline of secondary steel basin bottom is connected to the opening for feed of surge tank 5 one ends, the surge tank bottom is provided with the acid sludge relief outlet, and the top discharging pipeline of the surge tank the other end is connected with the middle part feeding line of dehydration tower 7; The dehydration tower top connects the vent line of waste water, and the discharging pipeline of bottom is connected with the feeding line at phenol treating tower 8 middle parts; Phenol treating tower cat head connects the discharging pipeline of phenol product, and the discharging pipeline of tower bottom is connected to the middle part feeding line of ortho-cresol treating tower 9; The discharging pipeline of the adjoining cresols product of ortho-cresol treating tower cat head, the bottom discharge pipeline is connected with the intermediate feed pipeline of M-and P-cresols treating tower 10; M-and P-cresols treating tower cat head connects the discharging pipeline of M-and P-cresols product, and the bottom connects the discharging pipeline of xylenol residue.
Adopt the operational condition of this device as follows: dephenolize slag tower 6 operational conditions are: the cat head working pressure is 10.0～25.0KPa, and reflux ratio is 0.5/1～1/1, and tower top temperature is 110.0～116.0 ℃, and column bottom temperature is 175.0～185.0 ℃; Dehydration tower 7 operational conditions are: the cat head working pressure is 10.0～25.0KPa,, reflux ratio is 0.5/1～1/1, and tower top temperature is 58.0～60.0 ℃, and column bottom temperature is 135.0～145.0 ℃; Phenol is refining to be taken 8 operational conditions and be: the cat head working pressure is 10.0～25.0KPa,, reflux ratio is 3/1～8/1, and tower top temperature is 120.0～125.0 ℃, and column bottom temperature is 150.0～155.0 ℃; Ortho-cresol treating tower 9 operational conditions are: the cat head working pressure is 10.0～25.0KPa, and reflux ratio is 3/1～6/1, and tower top temperature is 120.0～130.0 ℃, and column bottom temperature is 145.0～160.0 ℃; M-and P-cresols treating tower operational condition is: the cat head working pressure is 10.0～25.0KPa, and reflux ratio is 4/1～8/1, and tower top temperature is 135.0～140.0 ℃, and column bottom temperature is 155.0～165.0 ℃.
Concentrated acid is the sulphuric acid soln of 40.0～60.0wt%, and add-on is 3.0～5.0% of a crude phenols material quantity.Oxygenant is hydrogen peroxide or ozone, and add-on is 1.0～3.0% of a crude phenols amount.
Wherein dephenolize slag Tata internals are the valve tray structure, and all the other four Tata internals are efficient structured packing.
The device of whole separating technology is chosen to be 304 stainless steels, and the reboiler of each tower adopts thermosyphon reboiler.
(flow is 2500.0kg/h at the coal tar crude phenol stock liquid of certain coke-oven plant, component is a phenol 24.0%, ortho-cresol 16.0%, M-and P-cresols 20.0%, water 8.0%, xylenol 14.0%, heavy phenol 18.0%), at first its 3.0% sulphuric acid soln (40.0wt%) is entered the one-level static mixer together, add-on is 3.0% of a crude phenols raw material, carry out entering luwa evaporator behind the thorough mixing at the one-level steel basin with certain rotating speed then, after material enters dephenolize slag tower with gas phase, the bottom is discharged the phenol slag continuously, top distilled crude phenols raw material and hydrogen peroxide solution (30.0wt%) advance secondary steel basin and surge tank successively, its add-on is 1.0% of a crude phenols flow, acid sludge is discharged in the surge tank bottom, and crude phenols after treatment enter the phenol treating tower successively, ortho-cresol treating tower and M-and P-cresols treating tower.Dephenolize slag tower operational condition is: the cat head working pressure is 10.0KPa, and reflux ratio is 1/1, and tower top temperature is 110.0 ℃, and column bottom temperature is 175.0 ℃; Dehydration tower 7 operational conditions are: the cat head working pressure is 10.0KPa,, reflux ratio is 1/1, and tower top temperature is 58.0 ℃, and column bottom temperature is 135.0 ℃; Phenol treating tower 8 operational conditions are: the cat head working pressure is 10.0KPa,, reflux ratio is 3/1, and tower top temperature is 120.0 ℃, and column bottom temperature is 150.0 ℃; Ortho-cresol treating tower operational condition is: the cat head working pressure is 10.0KPa, and reflux ratio is 3/1, and tower top temperature is 120.0 ℃, and column bottom temperature is 145.0 ℃; M-and P-cresols treating tower operational condition is: the cat head working pressure is 10.0KPa, and reflux ratio is 4/1, and tower top temperature is 135.0 ℃, and column bottom temperature is 155.0 ℃.The technical target of the product that obtains is: phenol (quality product is 99.6wt%, and yield is 98.1%), ortho-cresol (quality product is 99.5wt%, and yield is 98.8%), M-and P-cresols (quality product is 99.1wt%, and yield is 97.8%).
Embodiment 2
(flow is 2980.0kg/h to the crude phenols stock liquid that reclaims in the brown coal pressurized gasification phenolic wastewater at certain factory of enterprise, component is a phenol 38.0%, ortho-cresol 10.0%, M-and P-cresols 28.0%, water 7.0%, xylenol 15.0%, heavy phenol 18.0%), at first it is entered the one-level static mixer with sulphuric acid soln (60.0wt%), add-on is 5.0% of a crude phenols raw material, carry out entering luwa evaporator behind the thorough mixing at the one-level steel basin with certain rotating speed then, after material enters dephenolize slag tower with gas phase, the bottom is discharged the phenol slag continuously, top distilled crude phenols raw material and hydrogen peroxide solution (30.0wt%) enter secondary steel basin and surge tank successively, add-on is 3.0% of a crude phenols raw material, acid sludge is discharged in the surge tank bottom, and crude phenols after treatment enter phenol tower successively, ortho-cresol tower and M-and P-cresols.Dephenolize slag tower operational condition is: the cat head working pressure is 12.0KPa, and reflux ratio is 0.8/1, and tower top temperature is 112.0 ℃, and column bottom temperature is 177.0 ℃; Dehydration tower 7 operational conditions are: the cat head working pressure is 12.0KPa,, reflux ratio is 0.6/1, and tower top temperature is 59.05 ℃, and column bottom temperature is 137.6 ℃; Phenol treating tower operational condition is: the cat head working pressure is 15.0KPa, and reflux ratio is 6/1, and tower top temperature is 123.0 ℃, and column bottom temperature is 153.0 ℃; Ortho-cresol treating tower operational condition is: the cat head working pressure is 15.0KPa, and reflux ratio is 4/1, and tower top temperature is 121.8 ℃, and column bottom temperature is 147.0 ℃; M-and P-cresols treating tower operational condition is: the cat head working pressure is 12.0KPa, and reflux ratio is 6/1, and tower top temperature is 136.9 ℃, and column bottom temperature is 157.8 ℃.The technical target of the product that obtains is: phenol (quality product is 99.6wt%, and yield is 98.2%), ortho-cresol (quality product is 99.5wt%, and yield is 99.2%), M-and P-cresols (quality product is 99.1wt%, and yield is 97.5%)
Coking crude phenols stock liquid (3000.0kg/h at certain coke-oven plant, component is a phenol 22.0%, ortho-cresol 14.0%, M-and P-cresols 18.0%, water 6.0%, xylenol 28.0%, heavy phenol 12.0%), at first it is entered the one-level static mixer with sulphuric acid soln (50.0wt%), add-on is that 4.0% of crude phenols raw material carries out entering luwa evaporator behind the thorough mixing at the one-level steel basin with certain rotating speed then, after material enters dephenolize slag tower with gas phase, the bottom is discharged the phenol slag continuously, top distilled crude phenols raw material and hydrogen peroxide solution (30.0wt%) enter secondary steel basin and surge tank successively, add-on is 2.0% of a crude phenols raw material, acid sludge is discharged in the surge tank bottom, and crude phenols after treatment enter the phenol treating tower successively, ortho-cresol treating tower and M-and P-cresols treating tower.Dephenolize slag tower operational condition is: the cat head working pressure is 25.0KPa, and reflux ratio is 0.5/1, and tower top temperature is 116.0 ℃, and column bottom temperature is 185.0.0 ℃; Dehydration tower 7 operational conditions are: the cat head working pressure is 25.0KPa, and reflux ratio is 0.8/1, and tower top temperature is 60.0 ℃, and column bottom temperature is 145.0 ℃; Phenol treating tower operational condition is: the cat head working pressure is 25.0KPa, and reflux ratio is 8/1, and tower top temperature is 125.0 ℃, and column bottom temperature is 155.0 ℃; Ortho-cresol treating tower operational condition is: the cat head working pressure is 25.0KPa, and reflux ratio is 6/1, and tower top temperature is 130.0 ℃, and column bottom temperature is 160.0 ℃; M-and P-cresols treating tower operational condition is: the cat head working pressure is 25.0KPa, and reflux ratio is 8/1, and tower top temperature is 140.0 ℃, and column bottom temperature is 165.0 ℃.The technical target of the product that obtains is: phenol (quality product is 99.6wt%, and yield is 98.1%), ortho-cresol (quality product is 99.5wt%, and yield is 99.2%), M-and P-cresols (quality product is 99.1wt%, and yield is 98.3%)
The tripping device and the method for a kind of coking crude phenols continuous rectification that the present invention proposes, be described by preferred embodiment, person skilled obviously can be in not breaking away from content of the present invention, spirit and scope to equipment as herein described and the preparation method changes or suitably change realize the technology of the present invention with combination.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.
Claims (10)
1. the continuous rectification tripping device of coking crude phenols is characterized in that comprising that the one-level pre-treatment that static mixer (1), one-level steel basin (2) and luwa evaporator (3) are formed adds acid unit; Comprise the secondary pre-treatment oxidation unit that secondary steel basin (4) and surge tank (5) are formed; Dephenolize slag tower (6) and comprise the essence slide Tower System of dehydration tower (7), phenol refining (8) tower, ortho-cresol tower (9) and M-and P-cresols tower (10); The one-level pre-treatment adds acid unit and connects dephenolize slag tower, and dephenolize slag tower connects secondary pre-treatment oxidation unit, and secondary pre-treatment oxidation unit connects the rectifying tower system.
2. the continuous rectification tripping device of coking crude phenols as claimed in claim 1, it is characterized in that crude phenols raw material and concentrated acid solution pipeline are connected to import one end that enters static mixer (1), the outlet of the static mixer the other end is connected to the inlet line on one-level steel basin (2) top, and the discharging pipeline of bottom directly is connected with the liquid phase feeding mouth on luwa evaporator (3) top; The upper, middle and lower portion of luwa evaporator (3) is provided with liquid phase feeding mouth, gas phase discharge port and acid sludge row mouth respectively, and the gas phase discharge port on top is connected to the feeding line at dephenolize slag tower (6) middle part; Dephenolize slag tower (6) cat head discharging pipeline and oxidant feed pipeline all are connected to the feeding line on secondary steel basin (4) top, the discharging pipeline of secondary steel basin bottom is connected to the opening for feed of surge tank (5) one ends, the surge tank bottom is provided with the acid sludge relief outlet, and the top discharging pipeline of the surge tank the other end is connected with the middle part feeding line of dehydration tower (7); The dehydration tower top connects the vent line of waste water, and the discharging pipeline of bottom is connected with the feeding line at phenol treating tower (8) middle part; The phenol tower cat head connects the discharging pipeline of phenol product, and the discharging pipeline of tower bottom is connected to the middle part feeding line of ortho-cresol tower (9); The discharging pipeline of the adjoining cresols product of ortho-cresol column overhead, the bottom discharge pipeline is connected with the intermediate feed pipeline of M-and P-cresols tower (10); The M-and P-cresols column overhead connects the discharging pipeline of M-and P-cresols product, and the bottom connects the discharging pipeline of xylenol residue.
3. the working method of the tripping device of claim 1 or a kind of coking crude phenols continuous rectification of 2 is characterized in that step is as follows:
1) crude phenols raw material and concentrated acid solution enter static mixer (1), and then enter one-level steel basin (2) and carry out entering luwa evaporator (3) after thorough mixing stirs, luwa evaporator (3) adopts external jacket formula steam heating, heavy constituent are discharged in the bottom, and the gaseous component on top enters dephenolize slag tower (6);
2) enter the crude phenols of dephenolize slag tower after dephenolize slag tower (6) is handled, dephenolize slag column overhead is to distillate crude phenols, heavy constituent are discharged in the bottom, taking off behind the slag crude phenols and oxygenant enters secondary steel basin (4) and carries out after mixed oxidization handles, enter surge tank (5) then, acid sludge is discharged in the surge tank bottom, and the cut that discharge at the top enters dehydration tower (7);
3) dehydration tower (7) top distillates the waste water that contains a small amount of phenol, and the cut of discharging at the bottom of the tower is to phenol treating tower (8); Phenol product is from phenol treating tower (8) extraction, and the cut that discharge phenol treating tower bottom is to ortho-cresol tower (9);
4) the ortho-cresol product is from ortho-cresol treating tower (9) cat head extraction, and the cut that discharge the bottom is to M-and P-cresols treating tower (10);
5) the M-and P-cresols product is from M-and P-cresols treating tower (10) cat head extraction, and the xylenol cut is discharged in the bottom.
4. working method as claimed in claim 3, it is characterized in that dephenolize slag tower (6) operational condition is: the cat head working pressure is 10.0～25.0KPa, and reflux ratio is 0.5/1～1/1, and tower top temperature is 110.0～116.0 ℃, and column bottom temperature is 175.0～185.0 ℃.
5. working method as claimed in claim 3, slag tower (7) operational condition that it is characterized in that dewatering is: the cat head working pressure is 10.0～25.0KPa,, reflux ratio is 0.5/1～1/1, and tower top temperature is 58.0～60.0 ℃, and column bottom temperature is 135.0～145.0 ℃.
6. working method as claimed in claim 3, it is characterized in that phenol treating tower (8) operational condition is: the cat head working pressure is 10.0～25.0KPa,, reflux ratio is 3/1～8/1, and tower top temperature is 120.0～125.0 ℃, and column bottom temperature is 150.0～155.0 ℃.
7. working method as claimed in claim 3, it is characterized in that ortho-cresol treating tower (9) operational condition is: the cat head working pressure is 10.0～25.0KPa, reflux ratio is 3/1～6/1, and tower top temperature is 120.0～130.0 ℃, and column bottom temperature is 145.0～155.0 ℃.
8. working method as claimed in claim 3, it is characterized in that M-and P-cresols treating tower (10) operational condition is: the cat head working pressure is 10.0～25.0KPa, reflux ratio is 4/1～8/1, and tower top temperature is 135.0～140.0 ℃, and column bottom temperature is 155.0～165.0 ℃.
9. working method as claimed in claim 3 is characterized in that described concentrated acid is the sulphuric acid soln of 40.0～60.0wt%, and add-on is 3.0～5.0% of a crude phenols material quantity.
10. working method as claimed in claim 3 is characterized in that described oxygenant is hydrogen peroxide or ozone, and add-on is 1.0～3.0% of a crude phenols amount.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910228047 CN101704726B (en) | 2009-11-06 | 2009-11-06 | Continuous refinement separation device and method of coked crude phenol |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910228047 CN101704726B (en) | 2009-11-06 | 2009-11-06 | Continuous refinement separation device and method of coked crude phenol |
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| Publication Number | Publication Date |
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| CN101704726A true CN101704726A (en) | 2010-05-12 |
| CN101704726B CN101704726B (en) | 2013-01-23 |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102125770A (en) * | 2010-12-15 | 2011-07-20 | 天津大学 | Continuous rectification device and method for treating heat-sensitive material by using wiped film evaporator |
| CN102153449A (en) * | 2011-03-15 | 2011-08-17 | 天津美科泰化工科技有限公司 | Continuous refining separation device and method for coal gasification crude phenol |
| CN102731264A (en) * | 2012-07-10 | 2012-10-17 | 陕西省石油化工研究设计院 | Method and device for continuously rectifying and separating medium/low-temperature coal tar crude phenols |
| CN102826962A (en) * | 2012-09-04 | 2012-12-19 | 李凤江 | Method and device for refining cumylphenol by using phenol tar |
| CN102826963A (en) * | 2012-09-04 | 2012-12-19 | 李凤江 | Method and device for producing p-cumylphenol by rectifying phenol oil tar |
| CN103709012A (en) * | 2013-11-22 | 2014-04-09 | 中建安装工程有限公司 | Industrialization processing method for tar crude phenols |
| CN105198711A (en) * | 2014-06-27 | 2015-12-30 | 上海宝钢化工有限公司 | Coked crude phenol refining device and method |
| CN105949037A (en) * | 2016-03-23 | 2016-09-21 | 中国科学院过程工程研究所 | Refining method of crude phenol from coking |
| CN106045822A (en) * | 2016-05-25 | 2016-10-26 | 长岭炼化岳阳工程设计有限公司 | Energy-saving phenol refining device with high product segmentation degree, and phenol refining method |
| CN107573219A (en) * | 2017-09-11 | 2018-01-12 | 赤峰博元科技有限公司 | A kind of improved refining of crude phenol system and method |
| CN109251130A (en) * | 2017-07-13 | 2019-01-22 | 鞍钢股份有限公司 | Process for producing 3, 5-xylenol at normal pressure by organic heat carrier heating technology |
| CN109251131A (en) * | 2017-07-13 | 2019-01-22 | 鞍钢股份有限公司 | Process for producing 3, 5-xylenol by organic heat carrier heating technology under reduced pressure |
| CN109628123A (en) * | 2019-01-23 | 2019-04-16 | 榆林市榆神工业区华航能源有限公司 | Coal tar dewatering |
| CN113511959A (en) * | 2020-04-10 | 2021-10-19 | 上海寰球工程有限公司 | System for separating phenol and acetophenone from tar |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102125770A (en) * | 2010-12-15 | 2011-07-20 | 天津大学 | Continuous rectification device and method for treating heat-sensitive material by using wiped film evaporator |
| CN102125770B (en) * | 2010-12-15 | 2013-04-24 | 天津大学 | Continuous rectification device and method for treating heat-sensitive material by using wiped film evaporator |
| CN102153449A (en) * | 2011-03-15 | 2011-08-17 | 天津美科泰化工科技有限公司 | Continuous refining separation device and method for coal gasification crude phenol |
| CN102153449B (en) * | 2011-03-15 | 2013-11-27 | 天津美科泰化工科技有限公司 | Continuous refining separation device and method for coal gasification crude phenol |
| CN102731264A (en) * | 2012-07-10 | 2012-10-17 | 陕西省石油化工研究设计院 | Method and device for continuously rectifying and separating medium/low-temperature coal tar crude phenols |
| CN102826962A (en) * | 2012-09-04 | 2012-12-19 | 李凤江 | Method and device for refining cumylphenol by using phenol tar |
| CN102826963A (en) * | 2012-09-04 | 2012-12-19 | 李凤江 | Method and device for producing p-cumylphenol by rectifying phenol oil tar |
| CN103709012A (en) * | 2013-11-22 | 2014-04-09 | 中建安装工程有限公司 | Industrialization processing method for tar crude phenols |
| CN105198711A (en) * | 2014-06-27 | 2015-12-30 | 上海宝钢化工有限公司 | Coked crude phenol refining device and method |
| CN105949037A (en) * | 2016-03-23 | 2016-09-21 | 中国科学院过程工程研究所 | Refining method of crude phenol from coking |
| CN105949037B (en) * | 2016-03-23 | 2019-01-25 | 中国科学院过程工程研究所 | A kind of coking crude phenol refining methd |
| CN106045822A (en) * | 2016-05-25 | 2016-10-26 | 长岭炼化岳阳工程设计有限公司 | Energy-saving phenol refining device with high product segmentation degree, and phenol refining method |
| CN109251130A (en) * | 2017-07-13 | 2019-01-22 | 鞍钢股份有限公司 | Process for producing 3, 5-xylenol at normal pressure by organic heat carrier heating technology |
| CN109251131A (en) * | 2017-07-13 | 2019-01-22 | 鞍钢股份有限公司 | Process for producing 3, 5-xylenol by organic heat carrier heating technology under reduced pressure |
| CN107573219A (en) * | 2017-09-11 | 2018-01-12 | 赤峰博元科技有限公司 | A kind of improved refining of crude phenol system and method |
| CN109628123A (en) * | 2019-01-23 | 2019-04-16 | 榆林市榆神工业区华航能源有限公司 | Coal tar dewatering |
| CN109628123B (en) * | 2019-01-23 | 2020-12-04 | 榆林市榆神工业区华航能源有限公司 | Coal tar dehydration process |
| CN113511959A (en) * | 2020-04-10 | 2021-10-19 | 上海寰球工程有限公司 | System for separating phenol and acetophenone from tar |
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