CN104628608B - A kind of tower negative pressure continuous noble gas air stripping blows naphthalene method and device thereof - Google Patents
A kind of tower negative pressure continuous noble gas air stripping blows naphthalene method and device thereof Download PDFInfo
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Abstract
The invention discloses a kind of tower negative pressure continuous noble gas air stripping and blow naphthalene method and device thereof, Multistage tower-type negative pressure continuous noble gas air stripping is used to blow naphthalene, blow compared with naphthalene technique with tradition, total energy consumption is the 30% of traditional handicraft, and owing to using noble gas to replace water vapour to carry out air stripping, noble gas not only obtains Efficient Cycle and utilizes, what is more important, blow naphthalene process to produce without waste water, from source, eliminate naphthalene water separate and the subsequent treatment operation of waste water, greatly reduce production cost;Simultaneously the present invention to blow naphthalene efficiency high, finally blow in the product after naphthalene containing naphthalene amount < 0.2%, be effectively increased the product quality of naphthalenes intermediate β LOMAR PWA EINECS 246-676-2, and blow the naphthalene time and shorten 2/3rds than traditional handicraft.It is simple that Multistage tower-type negative pressure blows naphthalene technological process continuously, and volume of equipment and quantity relatively traditional handicraft is greatly decreased, and effectively reduces Installed capital cost.The present invention effectively reduces entreprise cost and puts into, it is achieved energy-saving and emission-reduction, the production requirement of environmental protection.
Description
Technical field
The invention belongs to beta-naphthalenesulfonic-acid production technical field, be specifically related to a kind of tower negative pressure continuous noble gas air stripping and blow naphthalene method and device thereof.
Background technology
α-naphthalenesulfonicacid and beta-naphthalenesulfonic-acid are used as producing dyestuff, pesticide and the important intermediate of medicine, and the two is to prepare with naphthalene for the sulfonated reaction of raw material.The LOMAR PWA EINECS 246-676-2 using said method to produce may often be such that the mixture of its various isomers, α-naphthalenesulfonicacid is different due to its sulfonic group position from beta-naphthalenesulfonic-acid, performance there are differences, the production of some pesticide and medicine then needs highly purified beta-naphthalenesulfonic-acid, but even with the Optimum combinational scheme of beta-naphthalenesulfonic-acid synthesis condition, remain on and can inevitably synthesize a small amount of α-naphthalenesulfonicacid, need for this by-product α-naphthalenesulfonicacid present in reactant liquor after sulfonating reaction is hydrolyzed, the beta-naphthalenesulfonic-acid higher to obtaining purity.
The product obtained after the hydrolysis of sulfonating reaction mixture could obtain the purest beta-naphthalenesulfonic-acid after needing to carry out blowing naphthalene technique, at present, in commercial production, commonly used original steam distillation carries out blowing naphthalene, owing to steam temperature is different, naphthalene Gas content difference has different absorption gradients and partition coefficient to fresh naphthalene gas, existing simply blow naphthalene technique to blow naphthalene efficiency low, not only cause substantial amounts of steam consumption but also make that beta-naphthalenesulfonic-acid remains a certain amount of naphthalene and affect product quality, more seriously need substantial amounts of cooling water that naphthalene steam is flutterred collection for recovery naphthalene to reclaim, cause and produce waste water in a large number, increase disposal of three wastes difficulty.The means of production show, often produce 1 ton of beta-naphthalenesulfonic-acid, it it is 2.5 ~ 2.7 tons for blowing the quantity of steam of naphthalene, the cooling water inflow that these steam all condense needs is about 25 tons, the COD content of this waste water is at 1000 ~ 2000mg/L, and these waste water become the big environmental protection technical barrier that restriction beta-naphthalenesulfonic-acid produces.Meanwhile, using steam distillation to carry out blowing naphthalene energy consumption height, enterprise's production cost fall is not got off, it is difficult to realize energy-saving and emission-reduction, the target of cleaning production.
Summary of the invention
The first object of the present invention is to provide a kind of tower negative pressure continuous noble gas air stripping to blow naphthalene method, and the second purpose is to provide a kind of device realizing said method.
The first object of the present invention be achieved in that include one-level blow naphthalene, two grades blow naphthalene, three grades blow naphthalene, level Four blows naphthalene, Pyatyi blows naphthalene, concretely comprise the following steps:
A, one-level blows naphthalene: the hydrolyzed solution after sulfonating reaction mixture hydrolyzes in hydrolytic reaction pot blows naphthalene tower through heat exchanger entrance one-level, then blow the layer 5 column plate of naphthalene tower from one-level after hydrolyzed solution coordinates through blowing naphthalene tower with one-level tower bottoming cycle pump and tower bottom reboiler again to spray into one-level and blow naphthalene tower, noble gas blows naphthalene tower bottom through compressor from one-level from noble gas accumulator tank and contacts with hydrolyzed solution in a counter-current configuration, naphthalene steam and noble gas blow naphthalene top of tower from one-level and overflow into vaporization and condensation cooler, liquid phase naphthalene is sent into gas-liquid separator with noble gas from vaporization and condensation cooler and is separated, after separation, liquid phase naphthalene is pumped into refined naphthalene groove through naphtalene oil, noble gas is pumped into noble gas accumulator tank through ceramic vacuum, the hydrolyzed solution response time in one-level blows naphthalene tower is 60min;
B, two grades are blown naphthalene: the product after one-level blows naphthalene in step A blows naphthalene tower entrance two grades from one-level and blows naphthalene tower, described one-level blow naphthalene after the tower bottoming cycle pump that coordinates through blowing naphthalene tower with two grades of product and tower bottom reboiler after again spray into two grades from two grades of layer 5 column plates blowing naphthalene tower and blow naphthalene tower, noble gas blows naphthalene tower bottom through compressor from two grades from noble gas accumulator tank and blows the product after naphthalene in a counter-current configuration with one-level and contact, naphthalene steam and noble gas blow naphthalene top of tower from two grades and overflow into vaporization and condensation cooler, liquid phase naphthalene is sent into gas-liquid separator with noble gas from vaporization and condensation cooler and is separated, after separation, liquid phase naphthalene is pumped into refined naphthalene groove through naphtalene oil, noble gas is pumped into noble gas accumulator tank through ceramic vacuum, product after one-level blows naphthalene is 60min two grades of response time blown in naphthalene tower;
C, three grades are blown naphthalene: in step B two grades blow naphthalene after product blow naphthalene tower from two grades and enter three grades and blow naphthalene tower, described two grades blow naphthalene after the tower bottoming cycle pump that coordinates through blowing naphthalene tower with three grades of product and tower bottom reboiler after again spray into three grades from three grades of layer 5 column plates blowing naphthalene tower and blow naphthalene tower, noble gas blows product naphthalene tower bottom in a counter-current configuration with two grade blow naphthalene after through compressor from three grades from noble gas accumulator tank and contacts, naphthalene steam and noble gas blow naphthalene top of tower from three grades and overflow into vaporization and condensation cooler, liquid phase naphthalene is sent into gas-liquid separator with noble gas from vaporization and condensation cooler and is separated, after separation, liquid phase naphthalene is pumped into refined naphthalene groove through naphtalene oil, noble gas is pumped into noble gas accumulator tank through ceramic vacuum, two grades blow naphthalene after product be 60min three grades of response time blown in naphthalene tower;
D, level Four blows naphthalene: in step C three grades blow naphthalene after product blow naphthalene tower from three grades and enter level Four and blow naphthalene tower, described three grades blow naphthalene after the tower bottoming cycle pump that coordinates through blowing naphthalene tower with level Four of product and tower bottom reboiler after blow the layer 5 column plate of naphthalene tower from level Four and again spray into level Four and blow naphthalene tower, noble gas blows product naphthalene tower bottom in a counter-current configuration with three grade blow naphthalene after through compressor from level Four from noble gas accumulator tank and contacts, naphthalene steam and noble gas blow naphthalene top of tower from level Four and overflow into vaporization and condensation cooler, liquid phase naphthalene is sent into gas-liquid separator with noble gas from vaporization and condensation cooler and is separated, after separation, liquid phase naphthalene is pumped into refined naphthalene groove through naphtalene oil, noble gas is pumped into noble gas accumulator tank through ceramic vacuum, three grades blow naphthalene after product response time in level Four blows naphthalene tower be 60min;
E, Pyatyi blows naphthalene: the product after level Four blows naphthalene in step D blows naphthalene tower entrance Pyatyi from level Four and blows naphthalene tower, described level Four blow naphthalene after the tower bottoming cycle pump that coordinates through blowing naphthalene tower with Pyatyi of product and tower bottom reboiler after blow the layer 5 column plate of naphthalene tower from Pyatyi and again spray into Pyatyi and blow naphthalene tower, noble gas blows naphthalene tower bottom through compressor from Pyatyi from noble gas accumulator tank and blows the product after naphthalene in a counter-current configuration with level Four and contact, naphthalene steam and noble gas blow naphthalene top of tower from Pyatyi and overflow into vaporization and condensation cooler, liquid phase naphthalene is sent into gas-liquid separator with noble gas from vaporization and condensation cooler and is separated, after separation, liquid phase naphthalene is pumped into refined naphthalene groove through naphtalene oil, noble gas is pumped into noble gas accumulator tank through ceramic vacuum, product response time in Pyatyi blows naphthalene tower after level Four blows naphthalene is 60min.
The second object of the present invention is realized in, including hydrolytic reaction pot, heat exchanger, tower bottoming cycle pump, tower bottom reboiler, noble gas accumulator tank, gas-liquid separator, noble gas holding vessel, vaporization and condensation cooler, gas-liquid separator, refined naphthalene groove with blow naphthalene tower, described in blow naphthalene tower include one-level blow naphthalene tower, two grades blow naphthalene tower, three grades blow naphthalene tower, level Four is blown naphthalene tower Pyatyi and is blown naphthalene tower;It is characterized in that the discharging opening of described hydrolytic reaction pot is connected with the charging aperture of heat exchanger, the discharging opening of described heat exchanger blows the charging aperture of naphthalene tower and is connected with one-level, described one-level is blown naphthalene tower and is linked in sequence the tower bottoming cycle pump and tower bottom reboiler being matched therewith, described tower bottom reboiler connect respectively one-level blow naphthalene tower and two grades blow naphthalene tower;Described two grades are blown naphthalene tower and are linked in sequence the tower bottoming cycle pump and tower bottom reboiler being matched therewith, described tower bottom reboiler connect respectively two grades blow naphthalene tower and three grades blow naphthalene tower;Described three grades are blown naphthalene tower and are linked in sequence the tower bottoming cycle pump and tower bottom reboiler being matched therewith, and described tower bottom reboiler connects three grades respectively and blows naphthalene tower and blow naphthalene tower with level Four;Described level Four is blown naphthalene tower and is linked in sequence the tower bottoming cycle pump and tower bottom reboiler being matched therewith, and described tower bottom reboiler connects level Four respectively and blows naphthalene tower and blow naphthalene tower with Pyatyi;Described Pyatyi is blown naphthalene tower and is linked in sequence the tower bottoming cycle pump and tower bottom reboiler being matched therewith, and described tower bottom reboiler connects Pyatyi respectively and blows naphthalene tower and neutralize reactor;It is respectively provided with effusion meter on shower between the layer 5 column plate of what described connection tower bottom reboiler was matched therewith blow naphthalene tower, described connection tower bottom reboiler and next stage blow and are also provided with effusion meter on the conveying pipe of naphthalene tower, the air supply opening of described noble gas accumulator tank is connected with noble gas holding vessel, the gas outlet of described noble gas accumulator tank blow with one-level respectively after compressor naphthalene tower, two grades blow naphthalene tower, three grades blow naphthalene tower, level Four blows naphthalene tower and Pyatyi is blown the bottom air inlet of naphthalene tower and is connected;Described one-level blow naphthalene tower, two grades blow naphthalene tower, three grades blow naphthalene tower, level Four blows naphthalene tower and Pyatyi is blown the tower top gas outlet of the naphthalene tower air inlet all with vaporization and condensation cooler and is connected;The discharging opening of described condensate cooler is connected with the import of gas-liquid separator, and the gas outlet, top of described gas-liquid separator is connected with noble gas accumulator tank, and the bottom liquid outlet of described gas-liquid separator is connected with refined naphthalene groove by naphtalene oil pump.
The present invention steam distillation that breaks traditions carries out blowing the restriction of naphthalene method, Multistage tower-type negative pressure continuous noble gas air stripping is used to blow naphthalene, blow compared with naphthalene technique with tradition, total energy consumption is the 30% of traditional handicraft, and owing to using noble gas to replace water vapour to carry out air stripping, noble gas not only obtains Efficient Cycle and utilizes, what is more important, blow naphthalene process to produce without waste water, from source, eliminate naphthalene water separate and the subsequent treatment operation of waste water, greatly reduce production cost;Simultaneously the present invention to blow naphthalene efficiency high, finally blow in the product after naphthalene containing naphthalene amount < 0.2%, be effectively increased the product quality of naphthalenes intermediate beta-naphthalenesulfonic-acid, and blow the naphthalene time and shorten 2/3rds than traditional handicraft.It is simple that Multistage tower-type negative pressure blows naphthalene technological process continuously, and volume of equipment and quantity relatively traditional handicraft is greatly decreased, and public work amount is little, significantly reduces Installed capital cost.The present invention effectively reduces entreprise cost and puts into, it is achieved energy-saving and emission-reduction, the production requirement of environmental protection.
Accompanying drawing explanation
Fig. 1 is apparatus of the present invention structural representations;
In figure: 1-hydrolytic reaction pot, 2-heat exchanger, 3-one-level blows naphthalene tower, 31-bis-grades blows naphthalene tower, 32-tri-grades blows naphthalene tower, 33-level Four blows naphthalene tower, 34-Pyatyi blows naphthalene tower, 4-tower bottoming cycle pump, 5-tower bottom reboiler, 6-effusion meter, 7-noble gas accumulator tank, in 8-and reactor, 9-gas distributor, 10-noble gas holding vessel, 11-vaporization and condensation cooler, 12-steam generator, 13-gas-liquid separator, 14-naphtalene oil pump, 15-refined naphthalene groove, 16-ceramic vacuum pump, 17-compressor.
Detailed description of the invention
The present invention is further illustrated with embodiment below in conjunction with the accompanying drawings, but is any limitation as the present invention never in any form, based on present invention teach that any change or improvement made, belongs to protection scope of the present invention.
As it is shown in figure 1, the present invention provide tower negative pressure continuous noble gas air stripping blow naphthalene method, including one-level blow naphthalene, two grades blow naphthalene, three grades blow naphthalene, level Four blows naphthalene, Pyatyi blows naphthalene, concretely comprise the following steps:
nullA、One-level blows naphthalene: the hydrolyzed solution after sulfonating reaction mixture hydrolyzes in hydrolytic reaction pot 1 enters one-level through heat exchanger 2 and blows naphthalene tower 3,Then blow the layer 5 column plate of naphthalene tower 3 from one-level after hydrolyzed solution coordinates through blowing naphthalene tower 3 with one-level tower bottoming cycle pump 4 and tower bottom reboiler 5 again to spray into one-level and blow naphthalene tower 3,Noble gas blows from one-level through compressor 17 from noble gas accumulator tank 7 and contacts with hydrolyzed solution in a counter-current configuration bottom naphthalene tower 3,Naphthalene steam and noble gas blow naphthalene tower 3 top from one-level and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with noble gas from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Noble gas sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,The hydrolyzed solution response time in one-level blows naphthalene tower 3 is 60min;
nullB、Two grades are blown naphthalene: the product after one-level blows naphthalene in step A blows naphthalene tower 3 from one-level and enters two grades and blow naphthalene tower 31,Again spray into two grades from two grades of layer 5 column plates blowing naphthalene tower 31 after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 31 with two grades and tower bottom reboiler 5 and blow naphthalene tower 31,Noble gas blows from two grades through compressor 17 from noble gas accumulator tank 7 and blows the product after naphthalene bottom naphthalene tower 31 in a counter-current configuration with one-level and contact,Naphthalene steam and noble gas blow naphthalene tower 31 top from two grades and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with noble gas from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Noble gas sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Product after one-level blows naphthalene is 60min two grades of response time blown in naphthalene tower 31;
nullC、Three grades are blown naphthalene: in step B two grades blow naphthalene after product blow naphthalene tower 31 from two grades and enter three grades and blow naphthalene tower 32,Again spray into three grades from three grades of layer 5 column plates blowing naphthalene tower 32 after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 32 with three grades and tower bottom reboiler 5 and blow naphthalene tower 32,Noble gas contacts from three grades of products blown after blowing naphthalene with two grades in a counter-current configuration bottom naphthalene tower 32 through compressor 17 from noble gas accumulator tank 7,Naphthalene steam and noble gas blow naphthalene tower 32 top from three grades and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with noble gas from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Noble gas sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Two grades blow naphthalene after product be 60min three grades of response time blown in naphthalene tower 32;
nullD、Level Four blows naphthalene: in step C three grades blow naphthalene after product blow naphthalene tower 32 from three grades and enter level Four and blow naphthalene tower 33,Blow the layer 5 column plate of naphthalene tower 33 from level Four after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 33 with level Four and tower bottom reboiler 5 again to spray into level Four and blow naphthalene tower 33,The product that noble gas blows after blowing naphthalene with three grades in a counter-current configuration bottom naphthalene tower 33 from level Four through compressor 17 from noble gas accumulator tank 7 contacts,Naphthalene steam and noble gas blow naphthalene tower 33 top from level Four and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with noble gas from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Noble gas sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Three grades blow naphthalene after product response time in level Four blows naphthalene tower 33 be 60min;
nullE、Pyatyi blows naphthalene: the product after level Four blows naphthalene in step D blows naphthalene tower 33 from level Four and enters Pyatyi and blow naphthalene tower 34,Blow the layer 5 column plate of naphthalene tower 34 from Pyatyi after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 34 with Pyatyi and tower bottom reboiler 5 again to spray into Pyatyi and blow naphthalene tower 34,Noble gas blows from Pyatyi through compressor 17 from noble gas accumulator tank 7 and blows the product after naphthalene bottom naphthalene tower 34 in a counter-current configuration with level Four and contact,Naphthalene steam and noble gas blow naphthalene tower 34 top from Pyatyi and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with noble gas from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Noble gas sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Product response time in Pyatyi blows naphthalene tower 34 after level Four blows naphthalene is 60min.
In described step A, B, C, D, E, the tower tops blowing naphthalene tower at different levels keep the pressure of-10KPa ~-20KPa, 93 DEG C~the stripping temperature of 96 DEG C, and at the bottom of tower, holding 160 DEG C blows naphthalene temperature.
Sending into the noble gas blowing naphthalene tower at different levels in described step A, B, C, D, E is nitrogen, and the purity of described nitrogen is 99.999%.
The bottoms blowing naphthalene tower at different levels in described step A, B, C, D, E are provided with gas distributor 9.
A kind of tower negative pressure continuous noble gas air stripping that is applicable to that the present invention provides blows the device of naphthalene method, including hydrolytic reaction pot 1, heat exchanger 2, tower bottoming cycle pump 4, tower bottom reboiler 5, noble gas accumulator tank 7, gas-liquid separator 8, noble gas holding vessel 10, vaporization and condensation cooler 11, gas-liquid separator 13, refined naphthalene groove 15 with blow naphthalene tower, described in blow naphthalene tower and include that one-level is blown 3, two grades of naphthalene tower and blown that 31, three grades of naphthalene tower blows naphthalene tower 32, level Four is blown naphthalene tower 33 Pyatyi and blown naphthalene tower 34;The discharging opening of described hydrolytic reaction pot 1 is connected with the charging aperture of heat exchanger 2, the discharging opening of described heat exchanger 2 blows the charging aperture of naphthalene tower 3 and is connected with one-level, described one-level is blown naphthalene tower 3 and is linked in sequence the tower bottoming cycle pump 4 and tower bottom reboiler 5 being matched therewith, described tower bottom reboiler 5 connect respectively one-level blow naphthalene tower 3 and two grades blow naphthalene tower 31;Described two grades are blown naphthalene tower 31 and are linked in sequence the tower bottoming cycle pump 4 and tower bottom reboiler 5 being matched therewith, described tower bottom reboiler 5 connect respectively two grades blow naphthalene tower 31 and three grades blow naphthalene tower 32;Described three grades are blown naphthalene tower 32 and are linked in sequence the tower bottoming cycle pump 4 and tower bottom reboiler 5 being matched therewith, and described tower bottom reboiler 5 connects three grades respectively and blows naphthalene tower 32 and blow naphthalene tower 33 with level Four;Described level Four is blown naphthalene tower 33 and is linked in sequence the tower bottoming cycle pump 4 and tower bottom reboiler 5 being matched therewith, and described tower bottom reboiler 5 connects level Four respectively and blows naphthalene tower 33 and blow naphthalene tower 34 with Pyatyi;Described Pyatyi is blown naphthalene tower 34 and is linked in sequence the tower bottoming cycle pump 4 and tower bottom reboiler 5 being matched therewith, and described tower bottom reboiler 5 connects Pyatyi respectively and blows naphthalene tower 34 and neutralize reactor 8;It is respectively provided with effusion meter 6 on shower between the layer 5 column plate of what described connection tower bottom reboiler 5 was matched therewith blow naphthalene tower, described connection tower bottom reboiler 5 blows with next stage and is also provided with effusion meter 6 on the conveying pipe of naphthalene tower, the air supply opening of described noble gas accumulator tank 7 is connected with noble gas holding vessel 10, and the gas outlet of described noble gas accumulator tank 7 is blown 3, two grades of naphthalene tower after compressor 17 respectively and blown that 31, three grades of naphthalene tower blows naphthalene tower 32, level Four blows naphthalene tower 33 and Pyatyi is blown the bottom air inlet of naphthalene tower 34 and is connected with one-level;Described one-level is blown 3, two grades of naphthalene tower and is blown that 31, three grades of naphthalene tower blows naphthalene tower 32, level Four blows naphthalene tower 33 and Pyatyi is blown the tower top gas outlet of naphthalene tower 34 air inlet all with vaporization and condensation cooler 11 and is connected;The discharging opening of described condensate cooler 11 is connected with the import of gas-liquid separator 13, and the gas outlet, top of described gas-liquid separator 13 is connected with noble gas accumulator tank 7, and the bottom liquid outlet of described gas-liquid separator 13 is connected with refined naphthalene groove 15 by naphtalene oil pump 14.
Described one-level is blown 3, two grades of naphthalene tower and is blown that 31, three grades of naphthalene tower blows naphthalene tower 32, level Four blows naphthalene tower 33 and Pyatyi is blown the bottom of naphthalene tower 34 and is provided with gas distributor 9.
It is provided with ceramic vacuum pump 16 on pipeline between gas outlet, top and the noble gas accumulator tank 7 of described gas-liquid separator 13.
Between described effusion meter 6 and the tower bottom reboiler 5 being arranged on the shower connected between the layer 5 column plate blowing naphthalene tower that tower bottom reboiler 5 is matched therewith, flow control valve is set.
Described being arranged on connects tower bottom reboiler 5 and next stage and blows and arrange flow control valve between effusion meter 6 and the tower bottom reboiler 5 on the conveying pipe of naphthalene tower.
Embodiment
1
nullA、One-level blows naphthalene: the hydrolyzed solution after sulfonating reaction mixture hydrolyzes in hydrolytic reaction pot 1 enters one-level through heat exchanger 2 and blows naphthalene tower 3,Then blow the layer 5 column plate of naphthalene tower 3 from one-level after hydrolyzed solution coordinates through blowing naphthalene tower 3 with one-level tower bottoming cycle pump 4 and tower bottom reboiler 5 again to spray into one-level and blow naphthalene tower 3,Pure nitrogen gas blows from one-level through compressor 17 from noble gas accumulator tank 7 and contacts with hydrolyzed solution in a counter-current configuration bottom naphthalene tower 3,Naphthalene steam and nitrogen blow naphthalene tower 3 top from one-level and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen gas from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,The hydrolyzed solution response time in one-level blows naphthalene tower 3 is 60min;
nullB、Two grades are blown naphthalene: the product after one-level blows naphthalene in step A blows naphthalene tower 3 from one-level and enters two grades and blow naphthalene tower 31,Again spray into two grades from two grades of layer 5 column plates blowing naphthalene tower 31 after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 31 with two grades and tower bottom reboiler 5 and blow naphthalene tower 31,Nitrogen blows from two grades through compressor 17 from noble gas accumulator tank 7 and blows the product after naphthalene bottom naphthalene tower 31 in a counter-current configuration with one-level and contact,Naphthalene steam and nitrogen blow naphthalene tower 31 top from two grades and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Product after one-level blows naphthalene is 60min two grades of response time blown in naphthalene tower 31;
nullC、Three grades are blown naphthalene: in step B two grades blow naphthalene after product blow naphthalene tower 31 from two grades and enter three grades and blow naphthalene tower 32,Again spray into three grades from three grades of layer 5 column plates blowing naphthalene tower 32 after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 32 with three grades and tower bottom reboiler 5 and blow naphthalene tower 32,Nitrogen contacts from three grades of products blown after blowing naphthalene with two grades in a counter-current configuration bottom naphthalene tower 32 through compressor 17 from noble gas accumulator tank 7,Naphthalene steam and nitrogen blow naphthalene tower 32 top from three grades and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Two grades blow naphthalene after product be 60min three grades of response time blown in naphthalene tower 32;
nullD、Level Four blows naphthalene: in step C three grades blow naphthalene after product blow naphthalene tower 32 from three grades and enter level Four and blow naphthalene tower 33,Blow the layer 5 column plate of naphthalene tower 33 from level Four after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 33 with level Four and tower bottom reboiler 5 again to spray into level Four and blow naphthalene tower 33,The product that nitrogen blows after blowing naphthalene with three grades in a counter-current configuration bottom naphthalene tower 33 from level Four through compressor 17 from noble gas accumulator tank 7 contacts,Naphthalene steam and nitrogen blow naphthalene tower 33 top from level Four and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Three grades blow naphthalene after product response time in level Four blows naphthalene tower 33 be 60min;
nullE、Pyatyi blows naphthalene: the product after level Four blows naphthalene in step D blows naphthalene tower 33 from level Four and enters Pyatyi and blow naphthalene tower 34,Blow the layer 5 column plate of naphthalene tower 34 from Pyatyi after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 34 with Pyatyi and tower bottom reboiler 5 again to spray into Pyatyi and blow naphthalene tower 34,Nitrogen blows from Pyatyi through compressor 17 from noble gas accumulator tank 7 and blows the product after naphthalene bottom naphthalene tower 34 in a counter-current configuration with level Four and contact,Naphthalene steam and noble gas blow naphthalene tower 34 top from Pyatyi and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Product response time in Pyatyi blows naphthalene tower 34 after level Four blows naphthalene is 60min.
The purity being passed through the nitrogen blown in naphthalene tower at different levels in above-mentioned steps A, B, C, D, E is 99.999%, the tower tops blowing naphthalene tower the most at different levels keep the pressure of-10KPa, the stripping temperature of 93 DEG C, and at the bottom of tower, holding 160 DEG C blows naphthalene temperature, completing after Pyatyi blows naphthalene, in product is 0.19% containing naphthalene amount.
Embodiment
2
nullA、One-level blows naphthalene: the hydrolyzed solution after sulfonating reaction mixture hydrolyzes in hydrolytic reaction pot 1 enters one-level through heat exchanger 2 and blows naphthalene tower 3,Then blow the layer 5 column plate of naphthalene tower 3 from one-level after hydrolyzed solution coordinates through blowing naphthalene tower 3 with one-level tower bottoming cycle pump 4 and tower bottom reboiler 5 again to spray into one-level and blow naphthalene tower 3,Pure nitrogen gas blows from one-level through compressor 17 from noble gas accumulator tank 7 and contacts with hydrolyzed solution in a counter-current configuration bottom naphthalene tower 3,Naphthalene steam and nitrogen blow naphthalene tower 3 top from one-level and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen gas from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,The hydrolyzed solution response time in one-level blows naphthalene tower 3 is 60min;
nullB、Two grades are blown naphthalene: the product after one-level blows naphthalene in step A blows naphthalene tower 3 from one-level and enters two grades and blow naphthalene tower 31,Again spray into two grades from two grades of layer 5 column plates blowing naphthalene tower 31 after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 31 with two grades and tower bottom reboiler 5 and blow naphthalene tower 31,Nitrogen blows from two grades through compressor 17 from noble gas accumulator tank 7 and blows the product after naphthalene bottom naphthalene tower 31 in a counter-current configuration with one-level and contact,Naphthalene steam and nitrogen blow naphthalene tower 31 top from two grades and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Product after one-level blows naphthalene is 60min two grades of response time blown in naphthalene tower 31;
nullC、Three grades are blown naphthalene: in step B two grades blow naphthalene after product blow naphthalene tower 31 from two grades and enter three grades and blow naphthalene tower 32,Again spray into three grades from three grades of layer 5 column plates blowing naphthalene tower 32 after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 32 with three grades and tower bottom reboiler 5 and blow naphthalene tower 32,Nitrogen contacts from three grades of products blown after blowing naphthalene with two grades in a counter-current configuration bottom naphthalene tower 32 through compressor 17 from noble gas accumulator tank 7,Naphthalene steam and nitrogen blow naphthalene tower 32 top from three grades and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Two grades blow naphthalene after product be 60min three grades of response time blown in naphthalene tower 32;
nullD、Level Four blows naphthalene: in step C three grades blow naphthalene after product blow naphthalene tower 32 from three grades and enter level Four and blow naphthalene tower 33,Blow the layer 5 column plate of naphthalene tower 33 from level Four after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 33 with level Four and tower bottom reboiler 5 again to spray into level Four and blow naphthalene tower 33,The product that nitrogen blows after blowing naphthalene with three grades in a counter-current configuration bottom naphthalene tower 33 from level Four through compressor 17 from noble gas accumulator tank 7 contacts,Naphthalene steam and nitrogen blow naphthalene tower 33 top from level Four and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Three grades blow naphthalene after product response time in level Four blows naphthalene tower 33 be 60min;
nullE、Pyatyi blows naphthalene: the product after level Four blows naphthalene in step D blows naphthalene tower 33 from level Four and enters Pyatyi and blow naphthalene tower 34,Blow the layer 5 column plate of naphthalene tower 34 from Pyatyi after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 34 with Pyatyi and tower bottom reboiler 5 again to spray into Pyatyi and blow naphthalene tower 34,Nitrogen blows from Pyatyi through compressor 17 from noble gas accumulator tank 7 and blows the product after naphthalene bottom naphthalene tower 34 in a counter-current configuration with level Four and contact,Naphthalene steam and noble gas blow naphthalene tower 34 top from Pyatyi and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Product response time in Pyatyi blows naphthalene tower 34 after level Four blows naphthalene is 60min.
The purity being passed through the nitrogen blown in naphthalene tower at different levels in above-mentioned steps A, B, C, D, E is 99.999%, the tower tops blowing naphthalene tower the most at different levels keep the pressure of-15KPa, the stripping temperature of 95 DEG C, and at the bottom of tower, holding 160 DEG C blows naphthalene temperature, completing after Pyatyi blows naphthalene, in product is 0.18% containing naphthalene amount.
Embodiment
3
nullA、One-level blows naphthalene: the hydrolyzed solution after sulfonating reaction mixture hydrolyzes in hydrolytic reaction pot 1 enters one-level through heat exchanger 2 and blows naphthalene tower 3,Then blow the layer 5 column plate of naphthalene tower 3 from one-level after hydrolyzed solution coordinates through blowing naphthalene tower 3 with one-level tower bottoming cycle pump 4 and tower bottom reboiler 5 again to spray into one-level and blow naphthalene tower 3,Pure nitrogen gas blows from one-level through compressor 17 from noble gas accumulator tank 7 and contacts with hydrolyzed solution in a counter-current configuration bottom naphthalene tower 3,Naphthalene steam and nitrogen blow naphthalene tower 3 top from one-level and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen gas from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,The hydrolyzed solution response time in one-level blows naphthalene tower 3 is 60min;
nullB、Two grades are blown naphthalene: the product after one-level blows naphthalene in step A blows naphthalene tower 3 from one-level and enters two grades and blow naphthalene tower 31,Again spray into two grades from two grades of layer 5 column plates blowing naphthalene tower 31 after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 31 with two grades and tower bottom reboiler 5 and blow naphthalene tower 31,Nitrogen blows from two grades through compressor 17 from noble gas accumulator tank 7 and blows the product after naphthalene bottom naphthalene tower 31 in a counter-current configuration with one-level and contact,Naphthalene steam and nitrogen blow naphthalene tower 31 top from two grades and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Product after one-level blows naphthalene is 60min two grades of response time blown in naphthalene tower 31;
nullC、Three grades are blown naphthalene: in step B two grades blow naphthalene after product blow naphthalene tower 31 from two grades and enter three grades and blow naphthalene tower 32,Again spray into three grades from three grades of layer 5 column plates blowing naphthalene tower 32 after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 32 with three grades and tower bottom reboiler 5 and blow naphthalene tower 32,Nitrogen contacts from three grades of products blown after blowing naphthalene with two grades in a counter-current configuration bottom naphthalene tower 32 through compressor 17 from noble gas accumulator tank 7,Naphthalene steam and nitrogen blow naphthalene tower 32 top from three grades and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Two grades blow naphthalene after product be 60min three grades of response time blown in naphthalene tower 32;
nullD、Level Four blows naphthalene: in step C three grades blow naphthalene after product blow naphthalene tower 32 from three grades and enter level Four and blow naphthalene tower 33,Blow the layer 5 column plate of naphthalene tower 33 from level Four after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 33 with level Four and tower bottom reboiler 5 again to spray into level Four and blow naphthalene tower 33,The product that nitrogen blows after blowing naphthalene with three grades in a counter-current configuration bottom naphthalene tower 33 from level Four through compressor 17 from noble gas accumulator tank 7 contacts,Naphthalene steam and nitrogen blow naphthalene tower 33 top from level Four and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Three grades blow naphthalene after product response time in level Four blows naphthalene tower 33 be 60min;
nullE、Pyatyi blows naphthalene: the product after level Four blows naphthalene in step D blows naphthalene tower 33 from level Four and enters Pyatyi and blow naphthalene tower 34,Blow the layer 5 column plate of naphthalene tower 34 from Pyatyi after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 34 with Pyatyi and tower bottom reboiler 5 again to spray into Pyatyi and blow naphthalene tower 34,Nitrogen blows from Pyatyi through compressor 17 from noble gas accumulator tank 7 and blows the product after naphthalene bottom naphthalene tower 34 in a counter-current configuration with level Four and contact,Naphthalene steam and noble gas blow naphthalene tower 34 top from Pyatyi and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Product response time in Pyatyi blows naphthalene tower 34 after level Four blows naphthalene is 60min.
The purity being passed through the nitrogen blown in naphthalene tower at different levels in above-mentioned steps A, B, C, D, E is 99.999%, the tower tops blowing naphthalene tower the most at different levels keep the pressure of-20KPa, the stripping temperature of 96 DEG C, and at the bottom of tower, holding 160 DEG C blows naphthalene temperature, completing after Pyatyi blows naphthalene, in product is 0.15% containing naphthalene amount.
Embodiment
4
nullA、One-level blows naphthalene: the hydrolyzed solution after sulfonating reaction mixture hydrolyzes in hydrolytic reaction pot 1 enters one-level through heat exchanger 2 and blows naphthalene tower 3,Then blow the layer 5 column plate of naphthalene tower 3 from one-level after hydrolyzed solution coordinates through blowing naphthalene tower 3 with one-level tower bottoming cycle pump 4 and tower bottom reboiler 5 again to spray into one-level and blow naphthalene tower 3,Pure nitrogen gas blows from one-level through compressor 17 from noble gas accumulator tank 7 and contacts with hydrolyzed solution in a counter-current configuration bottom naphthalene tower 3,Naphthalene steam and nitrogen blow naphthalene tower 3 top from one-level and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen gas from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,The hydrolyzed solution response time in one-level blows naphthalene tower 3 is 60min;
nullB、Two grades are blown naphthalene: the product after one-level blows naphthalene in step A blows naphthalene tower 3 from one-level and enters two grades and blow naphthalene tower 31,Again spray into two grades from two grades of layer 5 column plates blowing naphthalene tower 31 after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 31 with two grades and tower bottom reboiler 5 and blow naphthalene tower 31,Nitrogen blows from two grades through compressor 17 from noble gas accumulator tank 7 and blows the product after naphthalene bottom naphthalene tower 31 in a counter-current configuration with one-level and contact,Naphthalene steam and nitrogen blow naphthalene tower 31 top from two grades and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Product after one-level blows naphthalene is 60min two grades of response time blown in naphthalene tower 31;
nullC、Three grades are blown naphthalene: in step B two grades blow naphthalene after product blow naphthalene tower 31 from two grades and enter three grades and blow naphthalene tower 32,Again spray into three grades from three grades of layer 5 column plates blowing naphthalene tower 32 after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 32 with three grades and tower bottom reboiler 5 and blow naphthalene tower 32,Nitrogen contacts from three grades of products blown after blowing naphthalene with two grades in a counter-current configuration bottom naphthalene tower 32 through compressor 17 from noble gas accumulator tank 7,Naphthalene steam and nitrogen blow naphthalene tower 32 top from three grades and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Two grades blow naphthalene after product be 60min three grades of response time blown in naphthalene tower 32;
nullD、Level Four blows naphthalene: in step C three grades blow naphthalene after product blow naphthalene tower 32 from three grades and enter level Four and blow naphthalene tower 33,Blow the layer 5 column plate of naphthalene tower 33 from level Four after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 33 with level Four and tower bottom reboiler 5 again to spray into level Four and blow naphthalene tower 33,The product that nitrogen blows after blowing naphthalene with three grades in a counter-current configuration bottom naphthalene tower 33 from level Four through compressor 17 from noble gas accumulator tank 7 contacts,Naphthalene steam and nitrogen blow naphthalene tower 33 top from level Four and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Three grades blow naphthalene after product response time in level Four blows naphthalene tower 33 be 60min;
nullE、Pyatyi blows naphthalene: the product after level Four blows naphthalene in step D blows naphthalene tower 33 from level Four and enters Pyatyi and blow naphthalene tower 34,Blow the layer 5 column plate of naphthalene tower 34 from Pyatyi after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 34 with Pyatyi and tower bottom reboiler 5 again to spray into Pyatyi and blow naphthalene tower 34,Nitrogen blows from Pyatyi through compressor 17 from noble gas accumulator tank 7 and blows the product after naphthalene bottom naphthalene tower 34 in a counter-current configuration with level Four and contact,Naphthalene steam and noble gas blow naphthalene tower 34 top from Pyatyi and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Product response time in Pyatyi blows naphthalene tower 34 after level Four blows naphthalene is 60min.
The purity being passed through the nitrogen blown in naphthalene tower at different levels in above-mentioned steps A, B, C, D, E is 99.999%, the tower tops blowing naphthalene tower the most at different levels keep the pressure of-10KPa, the stripping temperature of 96 DEG C, and at the bottom of tower, holding 160 DEG C blows naphthalene temperature, completing after Pyatyi blows naphthalene, in product is 0.175% containing naphthalene amount.
Embodiment
5
nullA、One-level blows naphthalene: the hydrolyzed solution after sulfonating reaction mixture hydrolyzes in hydrolytic reaction pot 1 enters one-level through heat exchanger 2 and blows naphthalene tower 3,Then blow the layer 5 column plate of naphthalene tower 3 from one-level after hydrolyzed solution coordinates through blowing naphthalene tower 3 with one-level tower bottoming cycle pump 4 and tower bottom reboiler 5 again to spray into one-level and blow naphthalene tower 3,Pure nitrogen gas blows from one-level through compressor 17 from noble gas accumulator tank 7 and contacts with hydrolyzed solution in a counter-current configuration bottom naphthalene tower 3,Naphthalene steam and nitrogen blow naphthalene tower 3 top from one-level and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen gas from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,The hydrolyzed solution response time in one-level blows naphthalene tower 3 is 60min;
nullB、Two grades are blown naphthalene: the product after one-level blows naphthalene in step A blows naphthalene tower 3 from one-level and enters two grades and blow naphthalene tower 31,Again spray into two grades from two grades of layer 5 column plates blowing naphthalene tower 31 after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 31 with two grades and tower bottom reboiler 5 and blow naphthalene tower 31,Nitrogen blows from two grades through compressor 17 from noble gas accumulator tank 7 and blows the product after naphthalene bottom naphthalene tower 31 in a counter-current configuration with one-level and contact,Naphthalene steam and nitrogen blow naphthalene tower 31 top from two grades and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Product after one-level blows naphthalene is 60min two grades of response time blown in naphthalene tower 31;
nullC、Three grades are blown naphthalene: in step B two grades blow naphthalene after product blow naphthalene tower 31 from two grades and enter three grades and blow naphthalene tower 32,Again spray into three grades from three grades of layer 5 column plates blowing naphthalene tower 32 after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 32 with three grades and tower bottom reboiler 5 and blow naphthalene tower 32,Nitrogen contacts from three grades of products blown after blowing naphthalene with two grades in a counter-current configuration bottom naphthalene tower 32 through compressor 17 from noble gas accumulator tank 7,Naphthalene steam and nitrogen blow naphthalene tower 32 top from three grades and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Two grades blow naphthalene after product be 60min three grades of response time blown in naphthalene tower 32;
nullD、Level Four blows naphthalene: in step C three grades blow naphthalene after product blow naphthalene tower 32 from three grades and enter level Four and blow naphthalene tower 33,Blow the layer 5 column plate of naphthalene tower 33 from level Four after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 33 with level Four and tower bottom reboiler 5 again to spray into level Four and blow naphthalene tower 33,The product that nitrogen blows after blowing naphthalene with three grades in a counter-current configuration bottom naphthalene tower 33 from level Four through compressor 17 from noble gas accumulator tank 7 contacts,Naphthalene steam and nitrogen blow naphthalene tower 33 top from level Four and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Three grades blow naphthalene after product response time in level Four blows naphthalene tower 33 be 60min;
nullE、Pyatyi blows naphthalene: the product after level Four blows naphthalene in step D blows naphthalene tower 33 from level Four and enters Pyatyi and blow naphthalene tower 34,Blow the layer 5 column plate of naphthalene tower 34 from Pyatyi after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 34 with Pyatyi and tower bottom reboiler 5 again to spray into Pyatyi and blow naphthalene tower 34,Nitrogen blows from Pyatyi through compressor 17 from noble gas accumulator tank 7 and blows the product after naphthalene bottom naphthalene tower 34 in a counter-current configuration with level Four and contact,Naphthalene steam and noble gas blow naphthalene tower 34 top from Pyatyi and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Product response time in Pyatyi blows naphthalene tower 34 after level Four blows naphthalene is 60min.
The purity being passed through the nitrogen blown in naphthalene tower at different levels in above-mentioned steps A, B, C, D, E is 99.999%, the tower tops blowing naphthalene tower the most at different levels keep the pressure of-20KPa, the stripping temperature of 93 DEG C, and at the bottom of tower, holding 160 DEG C blows naphthalene temperature, completing after Pyatyi blows naphthalene, in product is 0.18% containing naphthalene amount.
Embodiment
6
nullA、One-level blows naphthalene: the hydrolyzed solution after sulfonating reaction mixture hydrolyzes in hydrolytic reaction pot 1 enters one-level through heat exchanger 2 and blows naphthalene tower 3,Then blow the layer 5 column plate of naphthalene tower 3 from one-level after hydrolyzed solution coordinates through blowing naphthalene tower 3 with one-level tower bottoming cycle pump 4 and tower bottom reboiler 5 again to spray into one-level and blow naphthalene tower 3,Pure nitrogen gas blows from one-level through compressor 17 from noble gas accumulator tank 7 and contacts with hydrolyzed solution in a counter-current configuration bottom naphthalene tower 3,Naphthalene steam and nitrogen blow naphthalene tower 3 top from one-level and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen gas from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,The hydrolyzed solution response time in one-level blows naphthalene tower 3 is 60min;
nullB、Two grades are blown naphthalene: the product after one-level blows naphthalene in step A blows naphthalene tower 3 from one-level and enters two grades and blow naphthalene tower 31,Again spray into two grades from two grades of layer 5 column plates blowing naphthalene tower 31 after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 31 with two grades and tower bottom reboiler 5 and blow naphthalene tower 31,Nitrogen blows from two grades through compressor 17 from noble gas accumulator tank 7 and blows the product after naphthalene bottom naphthalene tower 31 in a counter-current configuration with one-level and contact,Naphthalene steam and nitrogen blow naphthalene tower 31 top from two grades and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Product after one-level blows naphthalene is 60min two grades of response time blown in naphthalene tower 31;
nullC、Three grades are blown naphthalene: in step B two grades blow naphthalene after product blow naphthalene tower 31 from two grades and enter three grades and blow naphthalene tower 32,Again spray into three grades from three grades of layer 5 column plates blowing naphthalene tower 32 after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 32 with three grades and tower bottom reboiler 5 and blow naphthalene tower 32,Nitrogen contacts from three grades of products blown after blowing naphthalene with two grades in a counter-current configuration bottom naphthalene tower 32 through compressor 17 from noble gas accumulator tank 7,Naphthalene steam and nitrogen blow naphthalene tower 32 top from three grades and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Two grades blow naphthalene after product be 60min three grades of response time blown in naphthalene tower 32;
nullD、Level Four blows naphthalene: in step C three grades blow naphthalene after product blow naphthalene tower 32 from three grades and enter level Four and blow naphthalene tower 33,Blow the layer 5 column plate of naphthalene tower 33 from level Four after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 33 with level Four and tower bottom reboiler 5 again to spray into level Four and blow naphthalene tower 33,The product that nitrogen blows after blowing naphthalene with three grades in a counter-current configuration bottom naphthalene tower 33 from level Four through compressor 17 from noble gas accumulator tank 7 contacts,Naphthalene steam and nitrogen blow naphthalene tower 33 top from level Four and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Three grades blow naphthalene after product response time in level Four blows naphthalene tower 33 be 60min;
nullE、Pyatyi blows naphthalene: the product after level Four blows naphthalene in step D blows naphthalene tower 33 from level Four and enters Pyatyi and blow naphthalene tower 34,Blow the layer 5 column plate of naphthalene tower 34 from Pyatyi after tower bottoming cycle pump 4 that described product coordinates through blowing naphthalene tower 34 with Pyatyi and tower bottom reboiler 5 again to spray into Pyatyi and blow naphthalene tower 34,Nitrogen blows from Pyatyi through compressor 17 from noble gas accumulator tank 7 and blows the product after naphthalene bottom naphthalene tower 34 in a counter-current configuration with level Four and contact,Naphthalene steam and noble gas blow naphthalene tower 34 top from Pyatyi and overflow into vaporization and condensation cooler 11,Liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation cooler 11 and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14,Nitrogen sends into noble gas accumulator tank 7 through ceramic vacuum pump 16,Product response time in Pyatyi blows naphthalene tower 34 after level Four blows naphthalene is 60min.
The purity being passed through the nitrogen blown in naphthalene tower at different levels in above-mentioned steps A, B, C, D, E is 99.999%, and one-level blows the pressure that the tower top of naphthalene tower 3 keeps-10KPa, the stripping temperature of 93 DEG C simultaneously, keep at the bottom of tower 160 DEG C blow naphthalene temperature, blowing the naphthalene time is 60min;Two grades of tower tops blowing naphthalene tower 31 keep the pressure of-20KPa, the stripping temperature of 93 DEG C, keep at the bottom of tower 160 DEG C blow naphthalene temperature, blowing the naphthalene time is 60min;Three grades of tower tops blowing naphthalene tower 32 keep the pressure of-20KPa, the stripping temperature of 93 DEG C, keep at the bottom of tower 160 DEG C blow naphthalene temperature, blowing the naphthalene time is 60min;Level Four blows the pressure that the tower top of naphthalene tower 33 keeps-20KPa, the stripping temperature of 93 DEG C, keep at the bottom of tower 160 DEG C blow naphthalene temperature, blowing the naphthalene time is 60min;Pyatyi blows the pressure that the tower top of naphthalene tower 34 keeps-20KPa, the stripping temperature of 93 DEG C, keep at the bottom of tower 160 DEG C blow naphthalene temperature, blowing the naphthalene time is 60min;Completing after Pyatyi blows naphthalene, in product is 0.17% containing naphthalene amount.
The tower negative pressure continuous noble gas air stripping that the present invention provides blows naphthalene method and device has good expansibility, can blow naphthalene progression by increase and decrease and the supporting naphthalene device that blows realizes expanding;In actual production process, can increase and decrease blow naphthalene progression according to the actual requirement blowing naphthalene rate, thus effective cost-effective input.
Claims (10)
1. one kind is applicable to tower negative pressure continuous noble gas air stripping and blows the device of naphthalene method, including hydrolytic reaction pot (1), heat exchanger (2), tower bottoming cycle pump (4), tower bottom reboiler (5), noble gas accumulator tank (7), gas-liquid separator (8), noble gas holding vessel (10), vaporization and condensation cooler (11), gas-liquid separator (13), refined naphthalene groove (15) with blow naphthalene tower, described in blow naphthalene tower include one-level blow naphthalene tower (3), two grades blow naphthalene tower (31), three grades blow naphthalene tower (32), level Four is blown naphthalene tower (33) Pyatyi and is blown naphthalene tower (34);It is characterized in that the discharging opening of described hydrolytic reaction pot (1) is connected with the charging aperture of heat exchanger (2), the discharging opening of described heat exchanger (2) blows the charging aperture of naphthalene tower (3) and is connected with one-level, described one-level is blown naphthalene tower (3) and is linked in sequence tower bottoming cycle pump (4) and tower bottom reboiler (5) being matched therewith, and described tower bottom reboiler (5) connects one-level respectively and blows naphthalene tower (3) and blow naphthalene tower (31) with two grades;Described two grades are blown naphthalene tower (31) and are linked in sequence tower bottoming cycle pump (4) and tower bottom reboiler (5) being matched therewith, and described tower bottom reboiler (5) connects two grades respectively and blows naphthalene tower (31) and blow naphthalene tower (32) with three grades;Described three grades are blown naphthalene tower (32) and are linked in sequence tower bottoming cycle pump (4) and tower bottom reboiler (5) being matched therewith, and described tower bottom reboiler (5) connects three grades respectively and blows naphthalene tower (32) and blow naphthalene tower (33) with level Four;Described level Four is blown naphthalene tower (33) and is linked in sequence tower bottoming cycle pump (4) and tower bottom reboiler (5) being matched therewith, and described tower bottom reboiler (5) connects level Four respectively and blows naphthalene tower (33) and blow naphthalene tower (34) with Pyatyi;Described Pyatyi is blown naphthalene tower (34) and is linked in sequence tower bottoming cycle pump (4) and tower bottom reboiler (5) being matched therewith, and described tower bottom reboiler (5) connects Pyatyi respectively and blows naphthalene tower (34) and neutralize reactor (8);It is respectively provided with effusion meter (6) on shower between the layer 5 column plate blowing naphthalene tower that described connection tower bottom reboiler (5) is matched therewith, described connection tower bottom reboiler (5) and next stage blow and are also provided with effusion meter (6) on the conveying pipe of naphthalene tower, the air supply opening of described noble gas accumulator tank (7) is connected with noble gas holding vessel (10), the gas outlet of described noble gas accumulator tank (7) blows naphthalene tower (3) after compressor (17) respectively with one-level, two grades are blown naphthalene tower (31), three grades are blown naphthalene tower (32), level Four is blown naphthalene tower (33) and is blown the bottom air inlet of naphthalene tower (34) with Pyatyi and be connected;Described one-level blow naphthalene tower (3), two grades blow naphthalene tower (31), three grades blow naphthalene tower (32), level Four blows naphthalene tower (33) and Pyatyi is blown the tower top gas outlet of naphthalene tower (34) air inlet all with vaporization and condensation cooler (11) and is connected;The discharging opening of described condensate cooler (11) is connected with the import of gas-liquid separator (13), the gas outlet, top of described gas-liquid separator (13) is connected with noble gas accumulator tank (7), and the bottom liquid outlet of described gas-liquid separator (13) is connected with refined naphthalene groove (15) by naphtalene oil pump (14).
Device the most according to claim 1, it is characterised in that described one-level blow naphthalene tower (3), two grades blow naphthalene tower (31), three grades blow naphthalene tower (32), level Four blows naphthalene tower (33) and Pyatyi is blown the bottom of naphthalene tower (34) and is provided with gas distributor (9).
Device the most according to claim 1, it is characterised in that be provided with ceramic vacuum pump (16) on the pipeline between gas outlet, top and the noble gas accumulator tank (7) of described gas-liquid separator (13).
Device the most according to claim 1, it is characterised in that described in be arranged between effusion meter (6) and the tower bottom reboiler (5) on the shower connected between tower bottom reboiler (5) the layer 5 column plate blowing naphthalene tower that is matched therewith and be provided with flow control valve.
Device the most according to claim 1, it is characterised in that described in be arranged on and connect tower bottom reboiler (5) and blow with next stage between the effusion meter (6) and the tower bottom reboiler (5) that carry on pipe of naphthalene tower, flow control valve is set.
Device the most according to claim 1, it is characterised in that with this device implement tower negative pressure continuous noble gas air stripping blow the method for naphthalene include one-level blow naphthalene, two grades blow naphthalene, three grades blow naphthalene, level Four blows naphthalene, Pyatyi blows naphthalene, concretely comprise the following steps:
nullA、One-level blows naphthalene: the hydrolyzed solution after sulfonating reaction mixture hydrolyzes in hydrolytic reaction pot (1) blows naphthalene tower (3) through heat exchanger (2) entrance one-level,Then blow the layer 5 column plate of naphthalene tower (3) from one-level after hydrolyzed solution coordinates through blowing naphthalene tower (3) with one-level tower bottoming cycle pump (4) and tower bottom reboiler (5) again to spray into one-level and blow naphthalene tower (3),Noble gas blows naphthalene tower (3) bottom through compressor (17) from one-level from noble gas accumulator tank (7) and contacts with hydrolyzed solution in a counter-current configuration,Naphthalene steam and noble gas blow naphthalene tower (3) top from one-level and overflow into vaporization and condensation cooler (11),Liquid phase naphthalene is sent into gas-liquid separator (13) with noble gas from vaporization and condensation cooler (11) and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove (15) through naphtalene oil pump (14),Noble gas sends into noble gas accumulator tank (7) through ceramic vacuum pump (16),The hydrolyzed solution time of staying in one-level blows naphthalene tower (3) is 60min;
nullB、Two grades are blown naphthalene: the product after one-level blows naphthalene in step A blows naphthalene tower (3) entrance two grades from one-level and blows naphthalene tower (31),Again spray into two grades from two grades of layer 5 column plates blowing naphthalene tower (31) after tower bottoming cycle pump (4) that described product coordinates through blowing naphthalene tower (31) with two grades and tower bottom reboiler (5) and blow naphthalene tower (31),Noble gas blows naphthalene tower (31) bottom through compressor (17) from two grades from noble gas accumulator tank (7) and blows the product after naphthalene in a counter-current configuration with one-level and contact,Naphthalene steam and noble gas blow naphthalene tower (31) top from two grades and overflow into vaporization and condensation cooler (11),Liquid phase naphthalene is sent into gas-liquid separator (13) with noble gas from vaporization and condensation cooler (11) and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove (15) through naphtalene oil pump (14),Noble gas sends into noble gas accumulator tank (7) through ceramic vacuum pump (16),Product after one-level blows naphthalene is 60min in the time of staying that two grades are blown in naphthalene tower (31);
nullC、Three grades are blown naphthalene: in step B two grades blow naphthalene after product blow naphthalene tower (31) from two grades and enter three grades and blow naphthalene tower (32),Again spray into three grades from three grades of layer 5 column plates blowing naphthalene tower (32) after tower bottoming cycle pump (4) that described product coordinates through blowing naphthalene tower (32) with three grades and tower bottom reboiler (5) and blow naphthalene tower (32),Noble gas blows product naphthalene tower (32) bottom in a counter-current configuration with two grade blow naphthalene after through compressor (17) from three grades from noble gas accumulator tank (7) and contacts,Naphthalene steam and noble gas blow naphthalene tower (32) top from three grades and overflow into vaporization and condensation cooler (11),Liquid phase naphthalene is sent into gas-liquid separator (13) with noble gas from vaporization and condensation cooler (11) and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove (15) through naphtalene oil pump (14),Noble gas sends into noble gas accumulator tank (7) through ceramic vacuum pump (16),Two grades blow naphthalene after product be 60min in the time of staying that three grades are blown in naphthalene tower (32);
nullD、Level Four blows naphthalene: in step C three grades blow naphthalene after product blow naphthalene tower (32) from three grades and enter level Four and blow naphthalene tower (33),Blow the layer 5 column plate of naphthalene tower (33) from level Four after tower bottoming cycle pump (4) that described product coordinates through blowing naphthalene tower (33) with level Four and tower bottom reboiler (5) again to spray into level Four and blow naphthalene tower (33),Noble gas blows product naphthalene tower (33) bottom in a counter-current configuration with three grade blow naphthalene after through compressor (17) from level Four from noble gas accumulator tank (7) and contacts,Naphthalene steam and noble gas blow naphthalene tower (33) top from level Four and overflow into vaporization and condensation cooler (11),Liquid phase naphthalene is sent into gas-liquid separator (13) with noble gas from vaporization and condensation cooler (11) and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove (15) through naphtalene oil pump (14),Noble gas sends into noble gas accumulator tank (7) through ceramic vacuum pump (16),Three grades blow naphthalene after product time of staying in level Four blows naphthalene tower (33) be 60min;
nullE、Pyatyi blows naphthalene: the product after level Four blows naphthalene in step D blows naphthalene tower (33) entrance Pyatyi from level Four and blows naphthalene tower (34),Blow the layer 5 column plate of naphthalene tower (34) from Pyatyi after tower bottoming cycle pump (4) that described product coordinates through blowing naphthalene tower (34) with Pyatyi and tower bottom reboiler (5) again to spray into Pyatyi and blow naphthalene tower (34),Noble gas blows naphthalene tower (34) bottom through compressor (17) from Pyatyi from noble gas accumulator tank (7) and blows the product after naphthalene in a counter-current configuration with level Four and contact,Naphthalene steam and noble gas blow naphthalene tower (34) top from Pyatyi and overflow into vaporization and condensation cooler (11),Liquid phase naphthalene is sent into gas-liquid separator (13) with noble gas from vaporization and condensation cooler (11) and is separated,After separation, liquid phase naphthalene sends into refined naphthalene groove (15) through naphtalene oil pump (14),Noble gas sends into noble gas accumulator tank (7) through ceramic vacuum pump (16),Product time of staying in Pyatyi blows naphthalene tower (34) after level Four blows naphthalene is 60min.
Device the most according to claim 1, it is characterised in that in described step A, B, C, D, E, the tower tops blowing naphthalene tower at different levels keep the pressure of-10KPa ~-20KPa, the stripping temperature of 93 DEG C ~ 96 DEG C, and at the bottom of tower, holding 160 DEG C blows naphthalene temperature.
Device the most according to claim 1, it is characterised in that sending into the noble gas blowing naphthalene tower at different levels in described step A, B, C, D, E is nitrogen.
Device the most according to claim 8, it is characterised in that the purity sending into the nitrogen blowing naphthalene tower at different levels in described step A, B, C, D, E is 99.999%.
Device the most according to claim 1, it is characterised in that the bottoms blowing naphthalene tower at different levels in described step A, B, C, D, E are provided with gas distributor (9).
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CN107252666B (en) * | 2017-07-12 | 2022-10-21 | 艾洛益(杭州)材料科技有限公司 | Steam-water separation outlet device applied to oxygen-free closed system under inert gas protection |
CN112595133A (en) * | 2020-12-24 | 2021-04-02 | 中冶焦耐(大连)工程技术有限公司 | Industrial naphthalene vaporization and condensation cooler and working method thereof |
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