CN104628608A

CN104628608A - Method and device for blowing naphthalene via gas stripping by using tower type negative pressure continuous inert gas

Info

Publication number: CN104628608A
Application number: CN201510082980.9A
Authority: CN
Inventors: 罗国林; 冯辉
Original assignee: Many Synthesis Chemical Co Ltds In Qujing
Current assignee: Many Synthesis Chemical Co Ltds In Qujing
Priority date: 2015-02-16
Filing date: 2015-02-16
Publication date: 2015-05-20
Anticipated expiration: 2035-02-16
Also published as: CN104628608B

Abstract

The invention discloses a method and a device for blowing naphthalene via gas stripping by using tower type negative pressure continuous inert gas. The multi-stage tower type negative pressure continuous inert gas is adopted for blowing naphthalene via gas stripping, the total energy consumption is 30% of that of the conventional technology by comparing with the conventional naphthalene blowing technology, the inert gas is used for replacing the water vapor for performing the gas stripping operation, the inert gas is effectively recycled, and more importantly, the waste water is not generated during the naphthalene blowing process, so that the naphthalene water separating process and the following processing process for the waste water can be eliminated from the source, and the production cost is greatly reduced; the naphthalene blowing efficiency is high, the naphthalene content in the final blowing naphthalene product is less than 0.2%, the product quality of beta-naphthalene sulfonic acid in the naphthalene intermediate is effectively raised, and the naphthalene blowing time is shortened by 2/3 compared with that of the conventional technology. The multi-stage tower type negative pressure continuous naphthalene blowing technology is simple in process, the device volume and the number are greatly reduced compared with those of the conventional technology, and the construction investment cost is effectively reduced. The enterprise cost is effectively reduced, and the production requirements of energy saving, emission reducing and environment protection are realized.

Description

The continuous rare gas element air lift of a kind of tower negative pressure blows naphthalene method and device thereof

Technical field

The invention belongs to beta-naphthalenesulfonic-acid production technical field, be specifically related to the continuous rare gas element air lift of a kind of tower negative pressure and blow naphthalene method and device thereof.

Background technology

α-naphthalenesulfonicacid and beta-naphthalenesulfonic-acid are the important intermediate being used as to produce dyestuff, agricultural chemicals and medicine, and the two is that raw material obtains through sulfonation reaction with naphthalene.The naphthene sulfonic acid adopting aforesaid method to produce is usually the mixture of its various isomer, α-naphthalenesulfonicacid from beta-naphthalenesulfonic-acid because its sulfonic group position is different, performance there are differences, the production of some agricultural chemicals and medicine then needs highly purified beta-naphthalenesulfonic-acid, even but adopt the Optimum combinational scheme of beta-naphthalenesulfonic-acid synthesis condition, also still a small amount of α-naphthalenesulfonicacid can inevitably be synthesized, need the by product α-naphthalenesulfonicacid existed in the reaction solution after to sulfonation reaction to be hydrolyzed, to obtaining the higher beta-naphthalenesulfonic-acid of purity for this reason.

The product obtained after the hydrolysis of sulfonation reaction mixture could obtain comparatively pure beta-naphthalenesulfonic-acid after needing to carry out blowing naphthalene technique, at present, original steam distillation is generally adopted to carry out blowing naphthalene in industrial production, because steam temperature is different, naphthalene Gas content difference has different absorption gradients and partition ratio to fresh naphthalene gas, existingly simply blow naphthalene technique to blow naphthalene efficiency low, not only cause a large amount of steam consumptions but also make residual a certain amount of naphthalene in beta-naphthalenesulfonic-acid affect quality product, more seriously a large amount of water coolants is needed to flutter collection recovery to naphthalene steam for reclaiming naphthalene, cause a large amount of factory effluent, increase disposal of three wastes difficulty.The production means show, often produce 1 ton of beta-naphthalenesulfonic-acid, it is 2.5 ~ 2.7 tons for blowing the quantity of steam of naphthalene, the cooling water inflow whole for these steam condensation needed is about 25 tons, the COD content of this waste water is at 1000 ~ 2000mg/L, and these waste water become the large green technology difficult problem that restriction beta-naphthalenesulfonic-acid is produced.Meanwhile, adopt steam distillation to carry out blowing naphthalene energy consumption high, enterprise's production cost can fall, and is difficult to the target realizing energy-saving and emission-reduction, cleaner production.

Summary of the invention

The first object of the present invention is to provide the continuous rare gas element air lift of a kind of tower negative pressure to blow naphthalene method, and the second object is to provide a kind of device realizing aforesaid method.

The first object of the present invention is achieved in that and comprises that one-level blows naphthalene, secondary blows naphthalene, three grades are blown naphthalene, level Four blows naphthalene, Pyatyi blows naphthalene, and concrete steps are:

A, one-level blows naphthalene: the hydrolyzed solution after sulfonation reaction mixture is hydrolyzed in hydrolytic reaction pot enters one-level through interchanger and blows naphthalene tower, then hydrolyzed solution again sprays into one-level blow naphthalene tower through blowing with one-level the layer 5 column plate blowing naphthalene tower from one-level after recycle pump at the bottom of the tower that naphthalene tower coordinates and tower bottom reboiler, rare gas element blows naphthalene tower bottom through compressor from one-level from rare gas element storage tanks and contacts with hydrolyzed solution in a counter-current configuration, naphthalene steam and rare gas element blow naphthalene top of tower from one-level and overflow and enter vaporization and condensation water cooler, liquid phase naphthalene is sent into gas-liquid separator with rare gas element from vaporization and condensation water cooler and is separated, after being separated, liquid phase naphthalene is pumped into refined naphthalene groove through naphtalene oil, rare gas element is pumped into rare gas element storage tanks through ceramic vacuum, hydrolyzed solution is 60min in the reaction times that one-level is blown in naphthalene tower,

B, secondary blows naphthalene: the product after one-level blows naphthalene in steps A blows naphthalene tower from one-level and enters secondary and blow naphthalene tower, product after described one-level blows naphthalene again sprays into secondary blow naphthalene tower through blowing with secondary the layer 5 column plate blowing naphthalene tower from secondary after recycle pump at the bottom of the tower that naphthalene tower coordinates and tower bottom reboiler, rare gas element blows naphthalene tower bottom through compressor from secondary from rare gas element storage tanks and blows the product after naphthalene in a counter-current configuration with one-level and contact, naphthalene steam and rare gas element blow naphthalene top of tower from secondary and overflow and enter vaporization and condensation water cooler, liquid phase naphthalene is sent into gas-liquid separator with rare gas element from vaporization and condensation water cooler and is separated, after being separated, liquid phase naphthalene is pumped into refined naphthalene groove through naphtalene oil, rare gas element is pumped into rare gas element storage tanks through ceramic vacuum, product after one-level blows naphthalene is 60min in the reaction times that secondary blows in naphthalene tower,

C, three grades are blown naphthalene: the product after secondary blows naphthalene in step B blows naphthalene tower from secondary and enters three grades and blow naphthalene tower, the layer 5 column plate that product after described secondary blows naphthalene blows naphthalene tower from three grades after blowing recycle pump at the bottom of the tower that naphthalene tower coordinates and tower bottom reboiler with three grades again sprays into three grades and blows naphthalene tower, rare gas element blows naphthalene tower bottom through compressor from three grades from rare gas element storage tanks and blows the product after naphthalene in a counter-current configuration with secondary and contact, naphthalene steam and rare gas element blow naphthalene top of tower from three grades and overflow and enter vaporization and condensation water cooler, liquid phase naphthalene is sent into gas-liquid separator with rare gas element from vaporization and condensation water cooler and is separated, after being separated, liquid phase naphthalene is pumped into refined naphthalene groove through naphtalene oil, rare gas element is pumped into rare gas element storage tanks through ceramic vacuum, product after secondary blows naphthalene is 60min in the reaction times that three grades are 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 product again spray into level Four blow naphthalene tower through blowing with level Four the layer 5 column plate blowing naphthalene tower from level Four after recycle pump at the bottom of the tower that naphthalene tower coordinates and tower bottom reboiler, rare gas element blows naphthalene tower bottom through compressor from level Four from rare gas element storage tanks and blows the product after naphthalene with three grades in a counter-current configuration and contact, naphthalene steam and rare gas element blow naphthalene top of tower from level Four and overflow and enter vaporization and condensation water cooler, liquid phase naphthalene is sent into gas-liquid separator with rare gas element from vaporization and condensation water cooler and is separated, after being separated, liquid phase naphthalene is pumped into refined naphthalene groove through naphtalene oil, rare gas element is pumped into rare gas element storage tanks through ceramic vacuum, three grades blow naphthalene after product be 60min in the reaction times that level Four is blown in naphthalene tower,

E, Pyatyi blows naphthalene: the product after level Four blows naphthalene in step D blows naphthalene tower from level Four and enters Pyatyi and blow naphthalene tower, product after described level Four blows naphthalene again sprays into Pyatyi blow naphthalene tower through blowing with Pyatyi the layer 5 column plate blowing naphthalene tower from Pyatyi after recycle pump at the bottom of the tower that naphthalene tower coordinates and tower bottom reboiler, rare gas element blows naphthalene tower bottom through compressor from Pyatyi from rare gas element storage tanks and blows the product after naphthalene in a counter-current configuration with level Four and contact, naphthalene steam and rare gas element blow naphthalene top of tower from Pyatyi and overflow and enter vaporization and condensation water cooler, liquid phase naphthalene is sent into gas-liquid separator with rare gas element from vaporization and condensation water cooler and is separated, after being separated, liquid phase naphthalene is pumped into refined naphthalene groove through naphtalene oil, rare gas element is pumped into rare gas element storage tanks through ceramic vacuum, product after level Four blows naphthalene is 60min in the reaction times that Pyatyi is blown in naphthalene tower.

The second object of the present invention realizes like this, comprise recycle pump at the bottom of hydrolytic reaction pot, interchanger, tower, tower bottom reboiler, rare gas element storage tanks, gas-liquid separator, rare gas element hold-up vessel, vaporization and condensation water cooler, gas-liquid separator, refined naphthalene groove and blow naphthalene tower, described in blow that naphthalene tower comprises that one-level blows naphthalene tower, secondary blows naphthalene tower, three grades are blown naphthalene tower, level Four blows naphthalene tower Pyatyi and blow naphthalene tower; It is characterized in that the discharge port of described hydrolytic reaction pot is connected with the opening for feed of interchanger, the opening for feed that discharge port and the one-level of described interchanger blow naphthalene tower is connected, described one-level is blown naphthalene tower and to be linked in sequence recycle pump and tower bottom reboiler at the bottom of the tower that matches with it, and described tower bottom reboiler connects one-level respectively and blows naphthalene tower and secondary blows naphthalene tower; Described secondary blows naphthalene tower and to be linked in sequence recycle pump and tower bottom reboiler at the bottom of the tower that matches with it, described tower bottom reboiler connect respectively secondary blow naphthalene tower and three grades blow naphthalene tower; Described three grades are blown naphthalene tower and to be linked in sequence recycle pump and tower bottom reboiler at the bottom of the tower that matches with it, and described tower bottom reboiler connects three grades respectively and blows naphthalene tower and level Four blows naphthalene tower; Described level Four is blown naphthalene tower and to be linked in sequence recycle pump and tower bottom reboiler at the bottom of the tower that matches with it, and described tower bottom reboiler connects level Four respectively and blows naphthalene tower and Pyatyi blows naphthalene tower; Described Pyatyi is blown naphthalene tower and to be linked in sequence recycle pump and tower bottom reboiler at the bottom of the tower that matches with it, and described tower bottom reboiler connects Pyatyi respectively and blows naphthalene tower and neutralization reaction still; Shower between the layer 5 column plate of what described connection tower bottom reboiler matched with it blow naphthalene tower all arranges under meter, the transfer lime that described connection tower bottom reboiler and next stage blow naphthalene tower also arranges under meter, the air feed port of described rare gas element storage tanks is connected with rare gas element hold-up vessel, and naphthalene tower is blown with one-level respectively in the air outlet of described rare gas element storage tanks after compressor, secondary blows naphthalene tower, three grades are blown naphthalene tower, level Four blows naphthalene tower and be connected with the bottom air inlet that Pyatyi blows naphthalene tower; Described one-level blows naphthalene tower, secondary blows naphthalene tower, three grades are blown naphthalene tower, level Four blows naphthalene tower and be all connected with the inlet mouth of vaporization and condensation water cooler with the tower top air outlet that Pyatyi blows naphthalene tower; The discharge port of described condensate cooler is connected with the import of gas-liquid separator, and the air outlet, top of described gas-liquid separator is connected with rare gas element storage tanks, and the bottom liquid outlet of described gas-liquid separator is connected with refined naphthalene groove by naphtalene oil pump.

The present invention's steam distillation that breaks traditions carries out blowing the restriction of naphthalene method, the continuous rare gas element air lift of Multistage tower-type negative pressure is adopted to blow naphthalene, compared with blowing naphthalene technique with tradition, total energy consumption is 30% of traditional technology, and owing to adopting rare gas element to replace water vapor to carry out air lift, rare gas element not only obtains Efficient Cycle and utilizes, what is more important, blow naphthalene process to produce without waste water, eliminate the subsequent disposal operation of the separation of naphthalene water and waste water from source, greatly reduce production cost; Simultaneously naphthalene efficiency of blowing of the present invention is high, finally to blow in the product after naphthalene containing naphthalene amount < 0.2%, effectively improves the quality product of naphthalenes intermediate beta-naphthalenesulfonic-acid, and blows the naphthalene time and shorten 2/3rds than traditional technology.It is simple that Multistage tower-type negative pressure blows naphthalene technical process continuously, and volume of equipment and quantity comparatively traditional technology significantly reduce, and general facilities amount is little, significantly reduces Installed capital cost.The present invention effectively reduces enterprise cost and drops into, and realizes the production requirement of energy-saving and emission-reduction, environmental protection.

Accompanying drawing explanation

Fig. 1 is apparatus of the present invention structural representations;

In figure: 1-hydrolytic reaction pot, 2-interchanger, 3-one-level blows naphthalene tower, 31-secondary blows naphthalene tower, 32-tri-grades blows naphthalene tower, 33-level Four blows naphthalene tower, 34-Pyatyi blows naphthalene tower, recycle pump at the bottom of 4-tower, 5-tower bottom reboiler, 6-under meter, 7-rare gas element storage tanks, 8-neutralization reaction still, 9-gas distributor, 10-rare gas element hold-up vessel, 11-vaporization and condensation water cooler, 12-vapour generator, 13-gas-liquid separator, 14-naphtalene oil pump, 15-refined naphthalene groove, 16-ceramic vacuum pump, 17-compressor.

Embodiment

Below in conjunction with drawings and Examples, the present invention is further illustrated, but limited the present invention never in any form, and any change done based on training centre of the present invention or improvement, all belong to protection scope of the present invention.

As shown in Figure 1, the continuous rare gas element air lift of tower negative pressure provided by the invention blows naphthalene method, comprises that one-level blows naphthalene, secondary blows naphthalene, three grades are blown naphthalene, level Four blows naphthalene, Pyatyi blows naphthalene, and concrete steps are:

A, one-level blows naphthalene: the hydrolyzed solution after sulfonation reaction mixture is hydrolyzed in hydrolytic reaction pot 1 enters one-level through interchanger 2 and blows naphthalene tower 3, then hydrolyzed solution again sprays into one-level blow naphthalene tower 3 through blowing with one-level the layer 5 column plate blowing naphthalene tower 3 from one-level after recycle pump 4 at the bottom of the tower that naphthalene tower 3 coordinates and tower bottom reboiler 5, rare gas element to blow bottom naphthalene tower 3 from one-level through compressor 17 from rare gas element storage tanks 7 and contacts with hydrolyzed solution in a counter-current configuration, naphthalene steam and rare gas element blow naphthalene tower 3 top from one-level and overflow and enter vaporization and condensation water cooler 11, liquid phase naphthalene is sent into gas-liquid separator 13 with rare gas element from vaporization and condensation water cooler 11 and is separated, after being separated, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14, rare gas element sends into rare gas element storage tanks 7 through ceramic vacuum pump 16, hydrolyzed solution is 60min in the reaction times that one-level is blown in naphthalene tower 3,

B, secondary blows naphthalene: the product after one-level blows naphthalene in steps A blows naphthalene tower 3 from one-level and enters secondary and blow naphthalene tower 31, described product again sprays into secondary blow naphthalene tower 31 through blowing with secondary the layer 5 column plate blowing naphthalene tower 31 from secondary after recycle pump 4 at the bottom of the tower that naphthalene tower 31 coordinates and tower bottom reboiler 5, rare gas element to blow from secondary through compressor 17 from rare gas element storage tanks 7 and blows the product after naphthalene in a counter-current configuration with one-level bottom naphthalene tower 31 and contact, naphthalene steam and rare gas element blow naphthalene tower 31 top from secondary and overflow and enter vaporization and condensation water cooler 11, liquid phase naphthalene is sent into gas-liquid separator 13 with rare gas element from vaporization and condensation water cooler 11 and is separated, after being separated, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14, rare gas element sends into rare gas element storage tanks 7 through ceramic vacuum pump 16, product after one-level blows naphthalene is 60min in the reaction times that secondary blows in naphthalene tower 31,

C, three grades are blown naphthalene: the product after secondary blows naphthalene in step B blows naphthalene tower 31 from secondary and enters three grades and blow naphthalene tower 32, the layer 5 column plate that described product blows naphthalene tower 32 from three grades after blowing recycle pump 4 at the bottom of the tower that naphthalene tower 32 coordinates and tower bottom reboiler 5 with three grades again sprays into three grades and blows naphthalene tower 32, rare gas element to blow from three grades through compressor 17 from rare gas element storage tanks 7 and blows the product after naphthalene in a counter-current configuration with secondary bottom naphthalene tower 32 and contact, naphthalene steam and rare gas element blow naphthalene tower 32 top from three grades and overflow and enter vaporization and condensation water cooler 11, liquid phase naphthalene is sent into gas-liquid separator 13 with rare gas element from vaporization and condensation water cooler 11 and is separated, after being separated, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14, rare gas element sends into rare gas element storage tanks 7 through ceramic vacuum pump 16, product after secondary blows naphthalene is 60min in the reaction times that three grades are blown in naphthalene tower 32,

D, 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, described product again sprays into level Four blow naphthalene tower 33 through blowing with level Four the layer 5 column plate blowing naphthalene tower 33 from level Four after recycle pump 4 at the bottom of the tower that naphthalene tower 33 coordinates and tower bottom reboiler 5, rare gas element to blow from level Four through compressor 17 from rare gas element storage tanks 7 and blows the product after naphthalene with three grades in a counter-current configuration bottom naphthalene tower 33 and contact, naphthalene steam and rare gas element blow naphthalene tower 33 top from level Four and overflow and enter vaporization and condensation water cooler 11, liquid phase naphthalene is sent into gas-liquid separator 13 with rare gas element from vaporization and condensation water cooler 11 and is separated, after being separated, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14, rare gas element sends into rare gas element storage tanks 7 through ceramic vacuum pump 16, three grades blow naphthalene after product be 60min in the reaction times that level Four is blown in naphthalene tower 33,

E, 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, described product again sprays into Pyatyi blow naphthalene tower 34 through blowing with Pyatyi the layer 5 column plate blowing naphthalene tower 34 from Pyatyi after recycle pump 4 at the bottom of the tower that naphthalene tower 34 coordinates and tower bottom reboiler 5, rare gas element to blow from Pyatyi through compressor 17 from rare gas element storage tanks 7 and blows the product after naphthalene in a counter-current configuration with level Four bottom naphthalene tower 34 and contact, naphthalene steam and rare gas element blow naphthalene tower 34 top from Pyatyi and overflow and enter vaporization and condensation water cooler 11, liquid phase naphthalene is sent into gas-liquid separator 13 with rare gas element from vaporization and condensation water cooler 11 and is separated, after being separated, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14, rare gas element sends into rare gas element storage tanks 7 through ceramic vacuum pump 16, product after level Four blows naphthalene is 60min in the reaction times that Pyatyi is blown in naphthalene tower 34.

In described steps A, B, C, D, E, the tower top blowing naphthalene tower at different levels keeps the pressure of-10KPa ~-20KPa, the stripping temperature of 93 DEG C ~ 96 DEG C, keep at the bottom of tower 160 DEG C blow naphthalene temperature.

Sending into the rare gas element blowing naphthalene tower at different levels in described steps A, B, C, D, E is nitrogen, and the purity of described nitrogen is 99.999%.

Bottoms of blowing naphthalene tower at different levels in described steps A, B, C, D, E are provided with gas distributor 9.

Provided by the inventionly a kind ofly be applicable to the device that the continuous rare gas element air lift of tower negative pressure blows naphthalene method, comprise recycle pump 4, tower bottom reboiler 5, rare gas element storage tanks 7, gas-liquid separator 8, rare gas element hold-up vessel 10, vaporization and condensation water cooler 11, gas-liquid separator 13, refined naphthalene groove 15 at the bottom of hydrolytic reaction pot 1, interchanger 2, tower and blow naphthalene tower, described in blow that naphthalene tower comprises that one-level blows naphthalene tower 3, secondary blows that 31, three grades, naphthalene tower blows naphthalene tower 32, level Four is blown naphthalene tower 33 Pyatyi and blown naphthalene tower 34; The discharge port of described hydrolytic reaction pot 1 is connected with the opening for feed of interchanger 2, the opening for feed that discharge port and the one-level of described interchanger 2 blow naphthalene tower 3 is connected, described one-level is blown naphthalene tower 3 and to be linked in sequence recycle pump 4 and tower bottom reboiler 5 at the bottom of the tower that matches with it, and described tower bottom reboiler 5 connects one-level respectively and blows naphthalene tower 3 and blow naphthalene tower 31 with secondary; Described secondary blows naphthalene tower 31 and to be linked in sequence recycle pump 4 and tower bottom reboiler 5 at the bottom of the tower that matches with it, described tower bottom reboiler 5 connect respectively secondary blow naphthalene tower 31 and three grades blow naphthalene tower 32; Described three grades are blown naphthalene tower 32 and to be linked in sequence recycle pump 4 and tower bottom reboiler 5 at the bottom of the tower that matches with it, 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 to be linked in sequence recycle pump 4 and tower bottom reboiler 5 at the bottom of the tower that matches with it, 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 to be linked in sequence recycle pump 4 and tower bottom reboiler 5 at the bottom of the tower that matches with it, and described tower bottom reboiler 5 connects Pyatyi respectively and blows naphthalene tower 34 and neutralization reaction still 8; Shower between the layer 5 column plate of what described connection tower bottom reboiler 5 matched with it blow naphthalene tower all arranges under meter 6, the transfer lime that described connection tower bottom reboiler 5 and next stage blow naphthalene tower also arranges under meter 6, the air feed port of described rare gas element storage tanks 7 is connected with rare gas element hold-up vessel 10, and naphthalene tower 3 is blown with one-level respectively in the air outlet of described rare gas element storage tanks 7 after compressor 17, secondary blows that 31, three grades, naphthalene tower blows naphthalene tower 32, level Four is blown naphthalene tower 33 and is connected with the bottom air inlet that Pyatyi blows naphthalene tower 34; Described one-level blows naphthalene tower 3, secondary blows that 31, three grades, naphthalene tower blows naphthalene tower 32, level Four is blown naphthalene tower 33 and is all connected with the inlet mouth of vaporization and condensation water cooler 11 with the tower top air outlet that Pyatyi blows naphthalene tower 34; The discharge port of described condensate cooler 11 is connected with the import of gas-liquid separator 13, and the air outlet, top of described gas-liquid separator 13 is connected with rare gas element storage tanks 7, and the bottom liquid outlet of described gas-liquid separator 13 is connected with refined naphthalene groove 15 by naphtalene oil pump 14.

The bottom that described one-level blows naphthalene tower 3, secondary blows that 31, three grades, naphthalene tower blows naphthalene tower 32, level Four blows naphthalene tower 33 and Pyatyi blows naphthalene tower 34 is provided with gas distributor 9.

Pipeline between the air outlet, top of described gas-liquid separator 13 and rare gas element storage tanks 7 is provided with ceramic vacuum pump 16.

Described being arranged between under meter 6 on the shower that connects between the layer 5 column plate blowing naphthalene tower that matches with it of tower bottom reboiler 5 and tower bottom reboiler 5 arranges flow control valve.

Described being arranged on connects tower bottom reboiler 5 and next stage and blows between under meter 6 on the transfer lime of naphthalene tower and tower bottom reboiler 5 and arrange flow control valve.

embodiment 1

A, one-level blows naphthalene: the hydrolyzed solution after sulfonation reaction mixture is hydrolyzed in hydrolytic reaction pot 1 enters one-level through interchanger 2 and blows naphthalene tower 3, then hydrolyzed solution again sprays into one-level blow naphthalene tower 3 through blowing with one-level the layer 5 column plate blowing naphthalene tower 3 from one-level after recycle pump 4 at the bottom of the tower that naphthalene tower 3 coordinates and tower bottom reboiler 5, pure nitrogen gas to blow bottom naphthalene tower 3 from one-level through compressor 17 from rare gas element storage tanks 7 and contacts with hydrolyzed solution in a counter-current configuration, naphthalene steam and nitrogen blow naphthalene tower 3 top from one-level and overflow and enter vaporization and condensation water cooler 11, liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen gas from vaporization and condensation water cooler 11 and is separated, after being separated, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14, nitrogen sends into rare gas element storage tanks 7 through ceramic vacuum pump 16, hydrolyzed solution is 60min in the reaction times that one-level is blown in naphthalene tower 3,

B, secondary blows naphthalene: the product after one-level blows naphthalene in steps A blows naphthalene tower 3 from one-level and enters secondary and blow naphthalene tower 31, described product again sprays into secondary blow naphthalene tower 31 through blowing with secondary the layer 5 column plate blowing naphthalene tower 31 from secondary after recycle pump 4 at the bottom of the tower that naphthalene tower 31 coordinates and tower bottom reboiler 5, nitrogen to blow from secondary through compressor 17 from rare gas element storage tanks 7 and blows the product after naphthalene in a counter-current configuration with one-level bottom naphthalene tower 31 and contact, naphthalene steam and nitrogen blow naphthalene tower 31 top from secondary and overflow and enter vaporization and condensation water cooler 11, liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation water cooler 11 and is separated, after being separated, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14, nitrogen sends into rare gas element storage tanks 7 through ceramic vacuum pump 16, product after one-level blows naphthalene is 60min in the reaction times that secondary blows in naphthalene tower 31,

C, three grades are blown naphthalene: the product after secondary blows naphthalene in step B blows naphthalene tower 31 from secondary and enters three grades and blow naphthalene tower 32, the layer 5 column plate that described product blows naphthalene tower 32 from three grades after blowing recycle pump 4 at the bottom of the tower that naphthalene tower 32 coordinates and tower bottom reboiler 5 with three grades again sprays into three grades and blows naphthalene tower 32, nitrogen to blow from three grades through compressor 17 from rare gas element storage tanks 7 and blows the product after naphthalene in a counter-current configuration with secondary bottom naphthalene tower 32 and contact, naphthalene steam and nitrogen blow naphthalene tower 32 top from three grades and overflow and enter vaporization and condensation water cooler 11, liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation water cooler 11 and is separated, after being separated, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14, nitrogen sends into rare gas element storage tanks 7 through ceramic vacuum pump 16, product after secondary blows naphthalene is 60min in the reaction times that three grades are blown in naphthalene tower 32,

D, 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, described product again sprays into level Four blow naphthalene tower 33 through blowing with level Four the layer 5 column plate blowing naphthalene tower 33 from level Four after recycle pump 4 at the bottom of the tower that naphthalene tower 33 coordinates and tower bottom reboiler 5, nitrogen to blow from level Four through compressor 17 from rare gas element storage tanks 7 and blows the product after naphthalene with three grades in a counter-current configuration bottom naphthalene tower 33 and contact, naphthalene steam and nitrogen blow naphthalene tower 33 top from level Four and overflow and enter vaporization and condensation water cooler 11, liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation water cooler 11 and is separated, after being separated, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14, nitrogen sends into rare gas element storage tanks 7 through ceramic vacuum pump 16, three grades blow naphthalene after product be 60min in the reaction times that level Four is blown in naphthalene tower 33,

E, 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, described product again sprays into Pyatyi blow naphthalene tower 34 through blowing with Pyatyi the layer 5 column plate blowing naphthalene tower 34 from Pyatyi after recycle pump 4 at the bottom of the tower that naphthalene tower 34 coordinates and tower bottom reboiler 5, nitrogen to blow from Pyatyi through compressor 17 from rare gas element storage tanks 7 and blows the product after naphthalene in a counter-current configuration with level Four bottom naphthalene tower 34 and contact, naphthalene steam and rare gas element blow naphthalene tower 34 top from Pyatyi and overflow and enter vaporization and condensation water cooler 11, liquid phase naphthalene is sent into gas-liquid separator 13 with nitrogen from vaporization and condensation water cooler 11 and is separated, after being separated, liquid phase naphthalene sends into refined naphthalene groove 15 through naphtalene oil pump 14, nitrogen sends into rare gas element storage tanks 7 through ceramic vacuum pump 16, product after level Four blows naphthalene is 60min in the reaction times that Pyatyi is blown in naphthalene tower 34.

The purity passing into the nitrogen blown in naphthalene tower at different levels in above-mentioned steps A, B, C, D, E is 99.999%, simultaneously the tower top blowing naphthalene tower at different levels keeps the pressure of-10KPa, the stripping temperature of 93 DEG C, keep at the bottom of tower 160 DEG C blow naphthalene temperature, complete after Pyatyi blows naphthalene, in product is 0.19% containing naphthalene amount.

embodiment 2

The purity passing into the nitrogen blown in naphthalene tower at different levels in above-mentioned steps A, B, C, D, E is 99.999%, simultaneously the tower top blowing naphthalene tower at different levels keeps the pressure of-15KPa, the stripping temperature of 95 DEG C, keep at the bottom of tower 160 DEG C blow naphthalene temperature, complete after Pyatyi blows naphthalene, in product is 0.18% containing naphthalene amount.

embodiment 3

The purity passing into the nitrogen blown in naphthalene tower at different levels in above-mentioned steps A, B, C, D, E is 99.999%, simultaneously the tower top blowing naphthalene tower at different levels keeps the pressure of-20KPa, the stripping temperature of 96 DEG C, keep at the bottom of tower 160 DEG C blow naphthalene temperature, complete after Pyatyi blows naphthalene, in product is 0.15% containing naphthalene amount.

embodiment 4

The purity passing into the nitrogen blown in naphthalene tower at different levels in above-mentioned steps A, B, C, D, E is 99.999%, simultaneously the tower top blowing naphthalene tower at different levels keeps the pressure of-10KPa, the stripping temperature of 96 DEG C, keep at the bottom of tower 160 DEG C blow naphthalene temperature, complete after Pyatyi blows naphthalene, in product is 0.175% containing naphthalene amount.

embodiment 5

The purity passing into the nitrogen blown in naphthalene tower at different levels in above-mentioned steps A, B, C, D, E is 99.999%, simultaneously the tower top blowing naphthalene tower at different levels keeps the pressure of-20KPa, the stripping temperature of 93 DEG C, keep at the bottom of tower 160 DEG C blow naphthalene temperature, complete after Pyatyi blows naphthalene, in product is 0.18% containing naphthalene amount.

embodiment 6

The purity passing into the nitrogen blown in naphthalene tower at different levels in above-mentioned steps A, B, C, D, E is 99.999%, and the tower top that simultaneously one-level blows naphthalene tower 3 keeps the pressure of-10KPa, 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; The tower top that secondary blows naphthalene tower 31 keeps 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; The tower top that level Four blows naphthalene tower 33 keeps 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; The tower top that Pyatyi blows naphthalene tower 34 keeps 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; Complete after Pyatyi blows naphthalene, in product is 0.17% containing naphthalene amount.

Tower negative pressure provided by the invention continuous rare gas element air lift blows naphthalene method and device has good expansibility, namely blows naphthalene progression by increase and decrease and the supporting naphthalene device that blows realizes expanding; In actual production process, can according to actual requirement of blowing naphthalene rate, naphthalene progression is blown in increase and decrease, thus effective cost-saving input.

Claims

1. the continuous rare gas element air lift of tower negative pressure blows a naphthalene method, it is characterized in that comprising that one-level blows naphthalene, secondary blows naphthalene, three grades are blown naphthalene, level Four blows naphthalene, Pyatyi blows naphthalene, and concrete steps are:

A, one-level blows naphthalene: the hydrolyzed solution of sulfonation reaction mixture in hydrolytic reaction pot (1) after hydrolysis enters one-level through interchanger (2) and blow naphthalene tower (3), then hydrolyzed solution again sprays into one-level blow naphthalene tower (3) through blowing with one-level the layer 5 column plate blowing naphthalene tower (3) from one-level after recycle pump (4) at the bottom of the tower that naphthalene tower (3) coordinates and tower bottom reboiler (5), rare gas element blows naphthalene tower (3) bottom through compressor (17) from one-level from rare gas element storage tanks (7) and contacts with hydrolyzed solution in a counter-current configuration, naphthalene steam and rare gas element blow naphthalene tower (3) top from one-level and overflow and enter vaporization and condensation water cooler (11), liquid phase naphthalene is sent into gas-liquid separator (13) with rare gas element from vaporization and condensation water cooler (11) and is separated, after being separated, liquid phase naphthalene sends into refined naphthalene groove (15) through naphtalene oil pump (14), rare gas element sends into rare gas element storage tanks (7) through ceramic vacuum pump (16), hydrolyzed solution is 60min in the one-level residence time of blowing in naphthalene tower (3),

B, secondary blows naphthalene: the product after one-level blows naphthalene in steps A blows naphthalene tower (3) from one-level and enters secondary and blow naphthalene tower (31), described product again sprays into secondary blow naphthalene tower (31) through blowing with secondary the layer 5 column plate blowing naphthalene tower (31) from secondary after recycle pump (4) at the bottom of the tower that naphthalene tower (31) coordinates and tower bottom reboiler (5), rare gas element blows naphthalene tower (31) bottom through compressor (17) from secondary from rare gas element storage tanks (7) and blows the product after naphthalene in a counter-current configuration with one-level and contact, naphthalene steam and rare gas element blow naphthalene tower (31) top from secondary and overflow and enter vaporization and condensation water cooler (11), liquid phase naphthalene is sent into gas-liquid separator (13) with rare gas element from vaporization and condensation water cooler (11) and is separated, after being separated, liquid phase naphthalene sends into refined naphthalene groove (15) through naphtalene oil pump (14), rare gas element sends into rare gas element storage tanks (7) through ceramic vacuum pump (16), product after one-level blows naphthalene is 60min in the secondary residence time of blowing in naphthalene tower (31),

C, three grades are blown naphthalene: the product after secondary blows naphthalene in step B blows naphthalene tower (31) from secondary and enters three grades and blow naphthalene tower (32), the layer 5 column plate that described product blows naphthalene tower (32) from three grades after blowing recycle pump (4) at the bottom of the tower that naphthalene tower (32) coordinates and tower bottom reboiler (5) with three grades again sprays into three grades and blows naphthalene tower (32), rare gas element blows naphthalene tower (32) bottom through compressor (17) from three grades from rare gas element storage tanks (7) and blows the product after naphthalene in a counter-current configuration with secondary and contact, naphthalene steam and rare gas element blow naphthalene tower (32) top from three grades and overflow and enter vaporization and condensation water cooler (11), liquid phase naphthalene is sent into gas-liquid separator (13) with rare gas element from vaporization and condensation water cooler (11) and is separated, after being separated, liquid phase naphthalene sends into refined naphthalene groove (15) through naphtalene oil pump (14), rare gas element sends into rare gas element storage tanks (7) through ceramic vacuum pump (16), product after secondary blows naphthalene is 60min in the residence time that three grades are blown in naphthalene tower (32),

D, 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), described product again sprays into level Four blow naphthalene tower (33) through blowing with level Four the layer 5 column plate blowing naphthalene tower (33) from level Four after recycle pump (4) at the bottom of the tower that naphthalene tower (33) coordinates and tower bottom reboiler (5), rare gas element blows naphthalene tower (33) bottom through compressor (17) from level Four from rare gas element storage tanks (7) and blows the product after naphthalene with three grades in a counter-current configuration and contact, naphthalene steam and rare gas element blow naphthalene tower (33) top from level Four and overflow and enter vaporization and condensation water cooler (11), liquid phase naphthalene is sent into gas-liquid separator (13) with rare gas element from vaporization and condensation water cooler (11) and is separated, after being separated, liquid phase naphthalene sends into refined naphthalene groove (15) through naphtalene oil pump (14), rare gas element sends into rare gas element storage tanks (7) through ceramic vacuum pump (16), three grades blow naphthalene after product be 60min in the level Four residence time of blowing in naphthalene tower (33),

E, 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), described product again sprays into Pyatyi blow naphthalene tower (34) through blowing with Pyatyi the layer 5 column plate blowing naphthalene tower (34) from Pyatyi after recycle pump (4) at the bottom of the tower that naphthalene tower (34) coordinates and tower bottom reboiler (5), rare gas element blows naphthalene tower (34) bottom through compressor (17) from Pyatyi from rare gas element storage tanks (7) and blows the product after naphthalene in a counter-current configuration with level Four and contact, naphthalene steam and rare gas element blow naphthalene tower (34) top from Pyatyi and overflow and enter vaporization and condensation water cooler (11), liquid phase naphthalene is sent into gas-liquid separator (13) with rare gas element from vaporization and condensation water cooler (11) and is separated, after being separated, liquid phase naphthalene sends into refined naphthalene groove (15) through naphtalene oil pump (14), rare gas element sends into rare gas element storage tanks (7) through ceramic vacuum pump (16), product after level Four blows naphthalene is 60min in the Pyatyi residence time of blowing in naphthalene tower (34).

2. the continuous rare gas element air lift of tower negative pressure according to claim 1 blows naphthalene method, it is characterized in that in described steps A, B, C, D, E, the tower top blowing naphthalene tower at different levels keeps the pressure of-10KPa ~-20KPa, the stripping temperature of 93 DEG C ~ 96 DEG C, keep at the bottom of tower 160 DEG C blow naphthalene temperature.

3. the continuous rare gas element air lift of tower negative pressure according to claim 1 blows naphthalene method, it is characterized in that sending into the rare gas element blowing naphthalene tower at different levels in described steps A, B, C, D, E is nitrogen.

4. the continuous rare gas element air lift of tower negative pressure according to claim 3 blows naphthalene method, it is characterized in that sending into purity of blowing the nitrogen of naphthalene tower at different levels in described steps A, B, C, D, E is 99.999%.

5. the continuous rare gas element air lift of tower negative pressure according to claim 1 blows naphthalene method, it is characterized in that the bottoms of blowing naphthalene tower at different levels in described steps A, B, C, D, E are provided with gas distributor (9).

6. one kind is applicable to the device that the continuous rare gas element air lift of tower negative pressure blows naphthalene method, comprise recycle pump (4), tower bottom reboiler (5), rare gas element storage tanks (7), gas-liquid separator (8), rare gas element hold-up vessel (10), vaporization and condensation water cooler (11), gas-liquid separator (13), refined naphthalene groove (15) at the bottom of hydrolytic reaction pot (1), interchanger (2), tower and blow naphthalene tower, described in blow that naphthalene tower comprises that one-level blows naphthalene tower (3), secondary blows naphthalene tower (31), three grades are blown naphthalene tower (32), level Four blows naphthalene tower (33) Pyatyi and blow naphthalene tower (34), it is characterized in that the discharge port of described hydrolytic reaction pot (1) is connected with the opening for feed of interchanger (2), the opening for feed that discharge port and the one-level of described interchanger (2) blow naphthalene tower (3) is connected, described one-level is blown naphthalene tower (3) and to be linked in sequence recycle pump (4) and tower bottom reboiler (5) at the bottom of the tower that matches with it, and described tower bottom reboiler (5) connects one-level respectively and blows naphthalene tower (3) and blow naphthalene tower (31) with secondary, described secondary blows naphthalene tower (31) and to be linked in sequence recycle pump (4) and tower bottom reboiler (5) at the bottom of the tower that matches with it, and described tower bottom reboiler (5) connects secondary respectively and blows naphthalene tower (31) and blow naphthalene tower (32) with three grades, described three grades are blown naphthalene tower (32) and to be linked in sequence recycle pump (4) and tower bottom reboiler (5) at the bottom of the tower that matches with it, 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 to be linked in sequence recycle pump (4) and tower bottom reboiler (5) at the bottom of the tower that matches with it, 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 to be linked in sequence recycle pump (4) and tower bottom reboiler (5) at the bottom of the tower that matches with it, and described tower bottom reboiler (5) connects Pyatyi respectively and blows naphthalene tower (34) and neutralization reaction still (8), shower between the layer 5 column plate blowing naphthalene tower that described connection tower bottom reboiler (5) is matched with it all arranges under meter (6), the transfer lime that described connection tower bottom reboiler (5) and next stage blow naphthalene tower also arranges under meter (6), the air feed port of described rare gas element storage tanks (7) is connected with rare gas element hold-up vessel (10), naphthalene tower (3) is blown respectively in the air outlet of described rare gas element storage tanks (7) after compressor (17) with one-level, secondary blows naphthalene tower (31), three grades are blown naphthalene tower (32), level Four is blown naphthalene tower (33) and is connected with the bottom air inlet that Pyatyi blows naphthalene tower (34), described one-level blows naphthalene tower (3), secondary blows naphthalene tower (31), three grades are blown naphthalene tower (32), level Four blows naphthalene tower (33) and be all connected with the inlet mouth of vaporization and condensation water cooler (11) with the tower top air outlet that Pyatyi blows naphthalene tower (34), the discharge port of described condensate cooler (11) is connected with the import of gas-liquid separator (13), the air outlet, top of described gas-liquid separator (13) is connected with rare gas element storage tanks (7), and the bottom liquid outlet of described gas-liquid separator (13) is connected with refined naphthalene groove (15) by naphtalene oil pump (14).

7. device according to claim 6, is characterized in that described one-level blows naphthalene tower (3), secondary blows naphthalene tower (31), three grades are blown naphthalene tower (32), level Four blows naphthalene tower (33) and bottom that Pyatyi blows naphthalene tower (34) is provided with gas distributor (9).

8. device according to claim 6, is characterized in that the pipeline between the air outlet, top of described gas-liquid separator (13) and rare gas element storage tanks (7) is provided with ceramic vacuum pump (16).

9. device according to claim 6, is arranged on described in it is characterized in that between under meter (6) on the shower that connects between tower bottom reboiler (5) the layer 5 column plate blowing naphthalene tower that matches with it and tower bottom reboiler (5) and is provided with flow control valve.

10. device according to claim 6, is arranged on described in it is characterized in that and connects tower bottom reboiler (5) and next stage and blow between under meter (6) on the transfer lime of naphthalene tower and tower bottom reboiler (5) and arrange flow control valve.