CN102267868B - Industrial production apparatus for trichloroethylene - Google Patents
Industrial production apparatus for trichloroethylene Download PDFInfo
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- CN102267868B CN102267868B CN 201010188455 CN201010188455A CN102267868B CN 102267868 B CN102267868 B CN 102267868B CN 201010188455 CN201010188455 CN 201010188455 CN 201010188455 A CN201010188455 A CN 201010188455A CN 102267868 B CN102267868 B CN 102267868B
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Abstract
The invention provides an industrial production apparatus for trichloroethylene. The apparatus is characterized in that: an acetylene air inlet pipeline and a chlorine gas air inlet pipeline are respectively connected with an inlet end of a chlorination tower; an outlet end of a crude tetrachloroethane tank is connected with an inlet of a tetrachloroethane tower; an outlet end of a material feeding preheater of a dehydrochlorination reactor is connected with an inlet end of a desorber; an outlet end of a desorption residue tank is connected with an inlet end of a low-boiler tower; an outlet end arranged on the lower portion of the low-boiler tower is respectively connected with an inlet end of a reboiler of the low-boiler tower and an inlet end of a trichloroethylene tower; an outlet end of a trichloroethylene residue tank is connected with an inlet end of a middle distillate tower; an outlet end arranged on the lower portion of the middle distillate tower is respectively connected with an inlet end of a reboiler of the middle distillate tower and an inlet end of a tetrachloroethylene tower; heat exchanging devices of each complete condenser and each end cooler adopt graphite parts dipped in modified phenol formaldehyde resin. The industrial production apparatus for the trichloroethylene has characteristics of reasonable structure, large production capacity, safe, stable and long-period operation, and the prepared trichloroethylene has high quality.
Description
Technical field
The invention provides a kind of improved trieline production equipment.
Background technology
At present, domestic trieline manufacturing enterprise's overwhelming majority employing " gas phase catalysis dehydrochlorination " is produced.Its simple production flow process is: chlorine, acetylene gas generate thick tetrachloroethane in chlorination tower, thick tetrachloroethane is vaporized after rectifying, dehydrochlorination generates trieline in the dehydrochlorination reaction device, then passes through a series of distillation operation, produces qualified trieline product.Because " gas phase catalysis dehydrochlorination " trieline production equipment is emerging in recent years production technique, in the process of domestic other trielines manufacturing enterprise operation, a series of defective and problem have all appearred, show that plant capacity is less than normal, be 1.0 ten thousand ton/years of left and right, energy consumption is higher; The unit equipment load is less; The heat comprehensive utilization of production equipment is relatively poor; The dielectric corrosion problem of each operation of production equipment is difficult to solve; Trieline product second-rate.
Summary of the invention
Technical problem to be solved by this invention is, a kind of industrial production apparatus for trichloroethylene is provided, and this plant capacity is large, can be safely, stablize long-term operation.
the present invention realizes like this, industrial production apparatus for trichloroethylene, it has the acetylene admission line to be connected with the chlorination tower entrance end respectively with the chlorine admission line, the chlorination tower exit end is connected with chlorination tower complete condenser entrance end, chlorination tower complete condenser exit end is connected with chlorination return tank entrance end and chlorination tower tail cooler entrance end respectively, chlorination tower tail cooler exit end is connected with chlorination return tank entrance end and gas-liquid separator entrance end respectively, the gas-liquid separator exit end is connected with the tail gas buffer entrance end, the tail gas buffer exit end is connected with the hydraulic jet pump entrance end, the hydraulic jet pump exit end is connected with chlorination tail tank entrance end, chlorination tail tank exit end is connected with chlorination afterbay entrance end, chlorination afterbay exit end is connected with the pressure pump entrance end, another entrance end of pressure pump exit end and hydraulic jet pump is connected, chlorination return tank exit end is connected with thick tetrachloroethane tank entrance end, thick tetrachloroethane tank exit end is connected with tetrachloroethane tower entrance end, tetrachloroethane tower lower part outlet end is connected with tetrachloroethane tower reboiler entrance end and smart tetrachloroethane tank entrance end respectively, tetrachloroethane tower reboiler exit end is connected with another entrance end of tetrachloroethane tower, tetrachloroethane top of tower exit end is connected with tetrachloroethane tower complete condenser entrance end, tetrachloroethane tower complete condenser exit end is connected with tetrachloroethane tower return tank entrance end and tetrachloroethane tower tail cooler entrance end respectively, tetrachloroethane tail cooler exit end is connected with tetrachloroethane tower return tank entrance end, essence tetrachloroethane tank exit end is connected with tetrachloroethane vaporizer entrance end, tetrachloroethane vaporizer exit end is connected with dehydrochlorination reaction device feed preheater entrance end, dehydrochlorination reaction device feed preheater exit end is connected with thermal oil preheater entrance end, thermal oil preheater exit end is connected with dehydrochlorination reaction device entrance end, dehydrochlorination reaction device exit end is connected with another entrance end of dehydrochlorination reaction device feed preheater, another exit end of dehydrochlorination reaction device feed preheater is connected with the desorption tower entrance end, desorption tower outlet at bottom end is connected with the desorption tower reboiler entrance end, another entrance end of desorption tower reboiler exit end and desorption tower is connected, desorption tower top exit end is connected with desorption tower complete condenser entrance end, desorption tower complete condenser exit end is connected with desorption tower return tank entrance end and Analytic Tower tail cooler entrance end respectively, Analytic Tower tail cooler exit end is connected with desorption tower return tank entrance end, desorb return tank exit end is connected with extraction-container flow container entrance end, extraction-container flow container exit end is connected with the low tower entrance end that boils, the low tower lower part outlet end that boils is connected with low tower reboiler entrance end and the trieline tower entrance end of boiling respectively, the low tower reboiler exit end that boils is connected with low another entrance end of tower that boils, the low top of tower exit end that boils is connected with the low tower complete condenser entrance end that boils, the low tower complete condenser exit end that boils reaches the low tower tail cooler entrance end that boils with the low tower return tank entrance end that boils respectively and is connected, the low tower tail cooler exit end that boils is connected with the low tower return tank entrance end that boils, trieline tower lower part outlet end is connected with trieline tower reboiler entrance end and trieline still flow container entrance end respectively, trieline tower reboiler exit end is connected with another entrance end of trieline tower, trieline tower top exit end is connected with trieline tower complete condenser entrance end, trieline tower complete condenser exit end is connected with trieline tower tail cooler entrance end and trieline tower return tank entrance end respectively, trieline tower tail cooler exit end is connected with trieline return tank entrance end, trieline return tank exit end respectively with another entrance end of trieline tower, trieline discharging cooler inlet end is connected, trieline still flow container exit end is connected with middle runnings tower entrance end, middle runnings tower lower part outlet end is connected with middle runnings tower reboiler entrance end and zellon tower entrance end respectively, middle runnings tower top exit end is connected with middle runnings tower complete condenser entrance end, middle runnings tower complete condenser exit end is connected with middle runnings tower tail cooler entrance end and middle runnings tower return tank entrance end respectively, middle runnings tower tail cooler exit end is connected with another entrance end of middle runnings tower return tank, middle runnings tower return tank exit end is connected with another entrance end of desorb tower reactor flow container, zellon tower lower part outlet end and zellon tower reboiler entrance end, zellon tower top exit end is connected with zellon tower complete condenser entrance end, zellon tower complete condenser exit end is connected with zellon tower return tank entrance end and zellon tail cooler entrance end respectively, zellon tail cooler exit end is connected with another entrance end of zellon tower return tank, described each complete condenser, the heat exchange device of each tail cooler adopts the graphite piece of modified phenolic resin impregnate with tallow.
Adopt the industrial production apparatus for trichloroethylene of said structure, rational in infrastructure, throughput is large, can be safely, stablize long-term operation.The trieline quality product of producing is high.
Description of drawings
Fig. 1 is the schematic diagram of the part of structure of the present invention.
Fig. 2 is the schematic diagram of another part of structure of the present invention.
Fig. 3 is the schematic diagram of the acetylene gas drying purification device structure in the present invention.
Fig. 4 is the schematic diagram of the dehydrochlorination reaction apparatus structure in the present invention.
Fig. 5 is the schematic diagram of the gas distributor structure in the present invention.
Fig. 6 is the A-A sectional view of Fig. 5.
Fig. 7 has represented the master, has propped up the assembly relation of distribution pipe.
Fig. 8 is the B-B sectional view of Fig. 5.
Embodiment
Further illustrate the present invention below in conjunction with accompanying drawing.
as shown in drawings, the present invention's industrial production apparatus for trichloroethylene, it has the acetylene admission line to be connected with chlorination tower 9 entrance ends respectively with the chlorine admission line, chlorination tower 9 exit end are connected with chlorination tower complete condenser 7 entrance ends, chlorination tower complete condenser 7 exit end are connected with chlorination return tank 8 entrance ends and chlorination tower tail cooler 6 entrance ends respectively, chlorination tower tail cooler 6 exit end are connected with chlorination return tank 8 entrance ends and gas-liquid separator 5 entrance ends respectively, gas-liquid separator 5 exit end are connected with tail gas buffer 4 entrance ends, tail gas buffer 4 exit end are connected with hydraulic jet pump 3 entrance ends, hydraulic jet pump 3 exit end are connected with chlorination tail tank 10 entrance ends, chlorination tail tank 10 exit end are connected with chlorination afterbay 1 entrance end, chlorination afterbay 1 exit end is connected with pressure pump 2 entrance ends, pressure pump 2 exit end are connected with hydraulic jet pump 3 another entrance ends, chlorination return tank 8 exit end are connected with thick tetrachloroethane tank 11 entrance ends, thick tetrachloroethane tank 11 exit end are connected with tetrachloroethane tower 12 entrance ends, tetrachloroethane tower 12 lower part outlet ends are connected with tetrachloroethane tower reboiler 13 entrance ends and smart tetrachloroethane tank 17 entrance ends respectively, tetrachloroethane tower reboiler 13 exit end are connected with another entrance end of tetrachloroethane tower 12, tetrachloroethane tower 12 top exit ends are connected with tetrachloroethane tower complete condenser 14 entrance ends, tetrachloroethane tower complete condenser 14 exit end are connected with tetrachloroethane tower return tank 16 entrance ends and tetrachloroethane tower tail cooler 15 entrance ends respectively, tetrachloroethane tail cooler 15 exit end are connected with tetrachloroethane tower return tank 16 entrance ends, essence tetrachloroethane tank (17) exit end is connected with tetrachloroethane vaporizer 18 entrance ends, tetrachloroethane vaporizer exit end is connected with dehydrochlorination reaction device feed preheater 21 entrance ends, dehydrochlorination reaction device feed preheater 21 exit end are connected with thermal oil preheater 19 entrance ends, thermal oil preheater 19 exit end are connected with dehydrochlorination reaction device 20 entrance ends, dehydrochlorination reaction device 20 exit end are connected with dehydrochlorination reaction device feed preheater 21 another entrance ends, dehydrochlorination reaction device feed preheater 21 another exit end are connected with desorption tower 22 entrance ends, desorption tower 22 outlet at bottom ends are connected with desorption tower reboiler (23) entrance end, desorption tower reboiler 23 exit end are connected with desorption tower 22 another entrance ends, desorption tower top exit end is connected with desorption tower complete condenser 24 entrance ends, desorption tower complete condenser exit end is connected with desorption tower return tank 26 entrance ends and Analytic Tower tail cooler 25 entrance ends respectively, Analytic Tower tail cooler 25 exit end are connected with desorption tower return tank 26 entrance ends, desorb return tank 26 exit end are connected with extraction-container flow container 27 entrance ends, extraction-container flow container 27 exit end are connected with low tower 28 entrance ends that boil, the low tower 28 lower part outlet ends that boil are connected with low tower reboiler 29 entrance ends and trieline tower 33 entrance ends of boiling respectively, the low tower reboiler exit end that boils is connected with low another entrance end of tower that boils, the low tower 28 top exit ends that boil are connected with low tower complete condenser 30 entrance ends that boil, low tower complete condenser 30 exit end that boil reach low tower tail cooler 31 entrance ends that boil with low tower return tank 32 entrance ends that boil respectively and are connected, low tower tail cooler 31 exit end that boil are connected with low tower return tank 32 entrance ends that boil, trieline tower 33 lower part outlet ends are connected with trieline tower reboiler 34 entrance ends and trieline still flow container 39 entrance ends respectively, trieline tower reboiler 34 exit end are connected with trieline tower 33 another entrance ends, trieline tower 33 top exit end are connected with trieline tower complete condenser 35 entrance ends, trieline tower complete condenser 35 exit end are connected with trieline tower tail cooler 36 entrance ends and trieline tower return tank 37 entrance ends respectively, trieline tower tail cooler 36 exit end are connected with trieline return tank 37 entrance ends, trieline return tank 37 exit end respectively with trieline tower 33 another entrance ends, trieline discharging water cooler 38 entrance ends are connected, trieline still flow container 39 exit end are connected with middle runnings tower 40 entrance ends, middle runnings tower 40 lower part outlet ends are connected with middle runnings tower reboiler 41 entrance ends and zellon tower 45 entrance ends respectively, middle runnings tower 40 top exit end are connected with middle runnings tower complete condenser 42 entrance ends, middle runnings tower complete condenser 42 exit end are connected with middle runnings tower tail cooler 43 entrance ends and middle runnings tower return tank 44 entrance ends respectively, middle runnings tower tail cooler 43 exit end are connected with middle runnings tower return tank 44 another entrance ends, middle runnings tower return tank 44 exit end are connected with desorb tower reactor flow container 27 another entrance ends, zellon tower 45 lower part outlet ends and zellon tower reboiler 46 entrance ends, zellon tower 45 top exit end are connected with zellon tower complete condenser 47 entrance ends, zellon tower complete condenser 47 exit end are connected with zellon tower return tank 49 entrance ends and zellon tail cooler 48 entrance ends respectively, zellon tail cooler 48 exit end are connected with zellon tower return tank 49 another entrance ends, described each complete condenser, the heat exchange device of each tail cooler adopts the graphite piece of modified phenolic resin impregnate with tallow.The structure of the heat exchange device of each complete condenser, each tail cooler is identical with existing graphite material.
the specific works process of the present invention's production equipment is, enter chlorination tower 9 from the acetylene of acetylene admission line with from the chlorine of chlorine admission line, after reacting in containing the mother liquor of catalyzer, gas phase enters chlorination tower complete condenser 7, enter chlorination tower return tank 8 after the preliminary condensation of recirculated water, uncooled gas phase enters chlorination tower tail cooler 6, liquid phase after the chilled brine deep condensation flows into chlorination tower return tank 8, noncondensable gas is evacuated to gas-liquid separator 5 by vacuum, the isolated liquid phase of gas-liquid separator 5 enters thick tetrachloroethane tank 11, gas phase enters tail gas buffer 4, tail gas in tail gas buffer enters hydraulic jet pump 3, utilize the change in flow of hydraulic jet pump to vacuumize, directly enter chlorination tail tank 10 from hydraulic jet pump water out, the water of tail tank flows into afterbay 1, the water of afterbay is recycled through processing again.Be delivered to tetrachloroethane tower 12 from the thick tetrachloroethane in thick tetrachloroethane tank 11; after tetrachloroethane tower reboiler 13 heating rectifying separation; in tower, the rising gas phase is through tetrachloroethane tower complete condenser 14 and recirculated water heat exchange; phlegma flows into tetrachloroethane return tank 16; uncooled gas phase enters tetrachloroethane tail cooler 15 and chilled brine heat exchange; liquid phase flows into tetrachloroethane return tank 16; noncondensable gas emptying under nitrogen protection; material in the tetrachloroethane return tank refluxes mostly, and a small amount of extraction is to finished pot.deliver to tetrachloroethane vaporizer 18 from the tetrachloroethane in smart tetrachloroethane tank 17, gas after vaporization enters dehydrochlorination reaction device feed preheater 21 and carries out heat exchange with dehydrochlorination reaction device 20 gas out, then to thermal oil preheater 19, enter dehydrochlorination reaction device 20 through heat-conducting oil heating after temperature required, enter desorption tower 22 after the reacted mixed gas of dehydrochlorination reaction device is through 21 coolings of dehydrochlorination reaction device feed preheater, in the interior rising gas phase of tower, condensable gas is after desorption tower complete condenser 24 use circulating water coolings, liquid phase enters desorption tower return tank 26, not solidifying gas phase enters desorption tower tail cooler 25, liquid phase flows into desorb return tank 26 after the chilled brine deep condensation, noncondensable gas can be delivered to hydrogen chloride absorption workshop section, material in the desorption tower return tank all is back to desorption tower 22, the desorption tower reboiler 23 that connects on desorption tower, give heating material, make a large amount of rising material steams is arranged in tower, thereby make desorb tower reactor liquid acidity qualified, desorb tower reactor material enters desorb tower reactor flow container 27, material in the stripping vessel flow container is delivered to the low tower 28 that boils, through low tower reboiler 29 heating of boiling, after rectifying separation, in tower, the rising gas phase is after low tower complete condenser 30 condensations of boiling, liquid phase enters the low tower return tank 32 that boils, uncondensed gas enters to hang down boils tower tail cooler 31 after the chilled brine heat exchange, liquid phase flows into the low tower return tank 32 that boils, noncondensable gas emptying under nitrogen protection.Material in the low tower return tank that boils refluxes mostly, and a small amount of extraction is to finished pot.Hang down and boil the tower reactor mass transport to trieline tower 33; through 34 heating of trieline tower reboiler; after rectifying separation; in tower, the rising gas phase is after trieline tower complete condenser 35 circulating water condensings; phlegma enters trieline tower return tank 37; not solidifying gas enters trieline tower tail cooler 36 after the chilled brine condensation; liquid phase enters trieline tower return tank 37; not solidifying gas emptying under nitrogen protection; trieline tower return tank inner condensat liquid is back to tower top; to finished pot, tower bottoms is delivered to trieline tower reactor flow container 39 to the tower top material through the side line extraction.mass transport in trieline tower reactor flow container 39 is to middle runnings tower 40, after material enters the middle runnings tower, through 41 heating of middle runnings tower reboiler, after rectifying separation, in tower, rising steam is after middle runnings tower complete condenser 42 and recirculated water heat exchange, phlegma enters middle runnings tower return tank 44, after solidifying gas phase enters middle runnings tower tail cooler 43 and chilled brine heat exchange, liquid phase flows into middle runnings tower return tank 44, non-condensable gas emptying under nitrogen protection, the part of middle runnings tower return tank inner condensat liquid is back to the middle runnings column overhead through pipeline, another part extraction is to desorb tower reactor flow container 27.the middle runnings tower bottoms is delivered to zellon tower 45, material in zellon tower 45 heats through zellon tower reboiler, after rectifying separation, in tower, rising steam is after zellon tower complete condenser 47 and recirculated water heat exchange, phlegma enters zellon tower return tank 49, after solidifying gas phase enters zellon tower tail cooler 48 and recirculated water heat exchange, liquid phase flows into zellon tower return tank 49, non-condensable gas emptying under nitrogen protection, the part of zellon tower return tank inner condensat liquid is back to the zellon column overhead through pipeline, another part extraction is to the zellon test tank, tower bottoms is delivered to residual liquid tank.
Each entrance end is connected by pipeline respectively with exit end.
The equipment such as pressure pump, hydraulic jet pump, chlorination tower, each rectifying tower, vaporizer, dehydrochlorination reaction device, each interchanger identical with existing corresponding device with principle of work.
Triolefin discharging water cooler 38 exit end are connected with the trieline test tank.
Zellon tower 45 lower part outlet ends also are connected with the residual liquid tank entrance end.
Zellon tower return tank 49 exit end are connected with zellon tower 45 entrance ends and zellon test tank entrance end through pipeline respectively.
as shown in Figure 3, described acetylene admission line is connected with chlorination tower 9 entrance ends through acetylene gas drying purification device 50, there is acetylene admission line 523 to be connected with acetylene compressor 51 entrance ends on acetylene gas drying purification device 50, acetylene compressor 51 exit end are connected with acetylene water cooler 52 entrance ends, acetylene cooler outlet end is connected with acetylene spray catcher 53 entrance ends, acetylene spray catcher top exit end is connected with the dry I tower of sulfuric acid 56 lower inlet ends, the dry I tower of sulfuric acid top exit end is connected with the dry II tower of sulfuric acid 59 lower inlet ends, the dry II tower of sulfuric acid top exit end is connected with the dry III tower of sulfuric acid 512 lower inlet ends, the dry III tower of sulfuric acid top exit end is connected with acetylene acid separator 515 entrance ends, acetylene acid separator top exit end is connected with acetylene adsorption tower 517 entrance ends, acetylene water cooler 52 another exit end are connected with moisture holding tank 54 entrance ends, acetylene spray catcher 53 lower part outlet ends are connected with moisture holding tank 54 entrance ends, vitriol oil storage tank 520 exit end are connected with vitriol oil transferpump 522 entrance ends, vitriol oil transferpump exit end is connected with concentrated sulfuric acid cooler 514 entrance ends, the concentrated sulfuric acid cooler exit end is connected with the dry III tower of sulfuric acid 512 upper inlet ends, the dry III tower of sulfuric acid 512 lower part outlet ends are connected with the dry II tower of sulfuric acid 59 lower inlet ends, the dry III tower of sulfuric acid 512 another lower part outlet ends are connected with the dry III tower of sulfuric acid sulfuric acid recycle pump 513 entrance ends, the dry III tower of sulfuric acid sulfuric acid recycle pump 513 exit end are connected with dilute sulphuric acid recirculation cooler 511 entrance ends, dilute sulphuric acid recirculation cooler 511 exit end are connected with the dry III tower of sulfuric acid 512 upper inlet ends, the dry II tower of sulfuric acid 59 lower part outlet ends are connected with the dry I tower of sulfuric acid 56 lower inlet ends, the dry II tower of sulfuric acid 59 another lower part outlet ends are connected with the dry II tower of sulfuric acid sulfuric acid recycle pump 510 entrance ends, the dry II tower of sulfuric acid sulfuric acid recycle pump 510 exit end are connected with another dilute sulphuric acid recirculation cooler 58 entrance ends, another dilute sulphuric acid recirculation cooler 58 exit end are connected with the dry II tower of sulfuric acid 59 upper inlet ends, the dry I tower of sulfuric acid 56 lower part outlet ends are connected with the dry I tower of sulfuric acid sulfuric acid recycle pump 57 entrance ends, the dry I tower of sulfuric acid sulfuric acid recycle pump 57 exit end are connected with the 3rd dilute sulphuric acid recirculation cooler 55 entrance ends, the 3rd dilute sulphuric acid recirculation cooler 55 exit end are connected with the dry I tower of sulfuric acid 56 upper inlet ends, the dry I tower of sulfuric acid 56 another lower part outlet ends are connected with dilute sulphuric acid storage tank 519, nitrogen buffer tank 521 is connected with acetylene adsorption tower 517 lower inlet ends through nitrogen electric heater 518.
the specific works process of dry decontamination device is, acetylene gas enters acetylene compressor 51, and to be compressed to that gaseous tension raises be 0.135 ~ 0.15Mpa, enter again acetylene water cooler 52 and be cooled to 2 ~ 5 ℃, cooled acetylene gas is after acetylene spray catcher 53 captures water smoke, enter the sulfuric acid drying of the dry I tower of sulfuric acid 56 use 88% left and right, enter again the sulfuric acid drying of the dry II tower of sulfuric acid 59 use 92% left and right, then the vitriol oil that enters the dry III tower of sulfuric acid 512 use 98% is further dry, last acetylene gas is after acetylene acid separator 515 captures acid mist, entering the acetylene adsorption tower further purifies, acetylene gas after processing is moisture at 60-70ppm, strong oxidizing property due to the vitriol oil, also removed in the lump other impurity in the acetylene gas, acetylene gas has been played dewatered, the dual function that purifies.And traditional acetylene gas drying purification method adopts cold method, namely with cool brine, acetylene is cooled to 0 ℃ of left and right.Acetylene gas is moisture only can be down to 200-300ppm, and the too low meeting of temperature freezes pipeline, threatens normally and produces.
During first the driving, the water in acetylene spray catcher 53 and moisture holding tank 54 is added by tap water pipeline.In normal productive process, the water of condensation that is got off by acetylene water cooler 52 and 53 condensations of acetylene spray catcher flows automatically respectively to moisture holding tank 54, then regularly is disposed to trench.
The specific works process of sulfuric acid drying is: be 98% the vitriol oil from the purity of vitriol oil storage tank 520, by vitriol oil transferpump 522 be delivered to concentrated sulfuric acid cooler 514 cooling after, deliver to the dry III tower 512 of sulfuric acid, when the sulfuric acid in the dry III tower 512 of sulfuric acid surpasses certain liquid level, overflow enters the dry II tower 59 of sulfuric acid, the sulfuric acid of the dry III tower of sulfuric acid 512 bottoms is delivered to dilute sulphuric acid recirculation cooler 511 by the dry III tower of sulfuric acid sulfuric acid recycle pump 513 and enters the dry III tower 512 of sulfuric acid after cooling, forms the acid circulation.Dry at sulfuric acid
When the sulfuric acid in tower 59 surpasses certain liquid level, overflow enters the dry I tower 56 of sulfuric acid, and sulfuric acid is dry
The sulfuric acid of tower 59 bottoms by the dry II tower of sulfuric acid sulfuric acid recycle pump 510 be delivered to another dilute sulphuric acid recirculation cooler 58 cooling after, enter the sulfuric acid drying
Tower 59 forms the acid circulation.The sulfuric acid of the dry I tower of sulfuric acid 56 bottoms by the dry I tower of sulfuric acid sulfuric acid recycle pump 57 be delivered to the 3rd dilute sulphuric acid recirculation cooler 55 cooling after, enter the dry I tower 56 of sulfuric acid, form the acid circulation.The sulfuric acid liquid level of the dry I tower of sulfuric acid 56 bottoms drains into dilute sulphuric acid storage tank 519 when reaching certain level value.The acid mist that acetylene acid separator 515 captures flow to sulfuric acid holding tank 516 certainly, and then is disposed to dilute sulphuric acid storage tank 519.During first the driving, the sulfuric acid in each sulfuric acid tower and acetylene acid separator 515 all will first be injected into the regulation liquid level by vitriol oil transferpump 522.
Nitrogen enters nitrogen buffer tank 521 through the nitrogen admission line, after 518 heating of nitrogen electric heater, enters acetylene adsorption tower 517.Each entrance end is connected by pipeline respectively with exit end.The structure of the equipment such as acetylene compressor, acetylene water cooler, acetylene spray catcher, each sulfuric acid tower, acetylene acid separator, acetylene adsorption tower, sulfuric acid cooler, nitrogen electric heater 518 is identical with existing corresponding device with principle of work.For improving cooling performance, can adopt two-stage acetylene water cooler, the exit end of elementary acetylene water cooler is connected with secondary acetylene cooler inlet end, and the exit end of secondary acetylene water cooler is connected with acetylene spray catcher 53 entrance ends.The acetylene adsorption tower adopts adsorbing tower with molecular sieve.
as shown in Figure 4, on described dehydrochlorination reaction device 20, at least 3 tetrachloroethane vaporizers 202 are arranged, also have the quantity dehydrochlorination reaction device 206 identical with the tetrachloroethane vaporizer, the import of each tetrachloroethane vaporizer is connected with feeding line 201 through valve respectively, the outlet of each tetrachloroethane vaporizer is connected through the import of valve with the dehydrochlorination reaction device respectively, the outlet of each dehydrochlorination reaction device is connected with discharging pipeline 209 through valve respectively, between the outlet of each dehydrochlorination reaction device also through valve, pipeline 208 is connected, between the import of each dehydrochlorination reaction device also through valve, another pipeline 205 is connected, pipeline, be connected by connection line 207 between another pipeline, the outlet of each tetrachloroethane vaporizer is also through valve, the 3rd pipeline 203 is connected.
On this dehydrochlorination reaction device, every tetrachloroethane vaporizer and dehydrochlorination reaction device are composed in series a group reaction system, simultaneously, connection by pipeline and valve is controlled, and the inlet line of every dehydrochlorination reaction device is that tetrachloroethane vaporizer outlet line and outlet line interconnect respectively.Like this, every tetrachloroethane vaporizer can with the series operation of arbitrary dehydrochlorination reaction device, and any two dehydrochlorination reaction devices can carry out series operation.Operation two group reaction systems during normal production, a group reaction system reserve namely opens two standby one.When a certain group reaction system dehydrochlorination reaction catalyst activity reduction to 50% is following, stop the operation of this group reaction system, open the 3rd group reaction system.For further utilizing the activity of the catalyzer in the dehydrochlorination reaction system of stopping, reduce the trieline unit consumption, with the dehydrochlorination reaction device outlet in the 3rd group reaction system connect with the dehydrochlorination reaction device import of stopping (the dehydrochlorination reaction device that namely reopens catalyst activity reduction) move.Like this, can take full advantage of the activity of dehydrochlorination catalyzer, both can guarantee the high yield of dehydrochlorination reaction, avoid again the waste of catalyzer.The outlet of each tetrachloroethane vaporizer also is connected through valve, the 4th pipeline 204 respectively.Dehydrochlorination reaction device by said structure, and the expansion of tetrachloroethane tower, desorption tower, low boil tower, trieline tower, middle distillate tower and zellon tower throughput, can make the present invention's industrial production apparatus for trichloroethylene reach the throughput of 4.0 ten thousand ton/years of trielines.
As Fig. 5-shown in Figure 8, on gas distributor in described chlorination tower 9, main distribution pipe 91 is arranged, main distribution pipe two ends are horizontally connected with short distribution pipe 92, middle part and are horizontally connected with the distribution pipe 94 of drawing money on credit, short distribution pipe, draw money on credit have between distribution pipe in distribution pipe 93 cross connection on main distribution pipe, have respectively one to discharge pore 101 in the vertical direction of main second circumference of distribution pipe tube wall, vertical direction both sides, be distributed with many row's distribution pipe production wells 301 on second circumference of each distribution pipe tube wall.
During use, after packing into gas distributor in chlorination tower, at the two ends of each distribution pipe, closure plate 95 is installed, and is fixed on by U-bolt 910 on the fabricated section of acetylene chlorination tower inwall.At the end of main distribution pipe, another closure plate 96 is installed, and is fixed on the fabricated section of acetylene chlorination tower inwall by another U-bolt 911.Each distribution pipe can pass main distribution pipe, has through hole 302 to communicate with main distribution pipe inner chamber on a distribution pipe.The nut 98 that passes the bolt 97 of main a, distribution pipe and bolt two ends will be led, a distribution pipe is fixed together.Gas enters from the port 99 that main distribution pipe is exposed at acetylene chlorination tower outside, and the production well on each pipe is distributed in the acetylene chlorination tower.The gas distributor of this structure has improved chlorine, its distribution effect in chlorination mother solution of acetylene, obviously strengthened the distribution effect of gas, improved the yield of chlorination reaction, the purity of thick tetrachloroethane remains on 97-98%, exceeds 3-4% than the domestic same industry.Prevented because of skewness, reacted not exclusively, acetylene gas contacts the phenomenon of blasting with chlorine.
Trieline tower complete condenser shell side, trieline discharging water cooler shell side, trieline test tank, trieline storage tank material are replaced by stainless steel by carbon steel, guaranteed that effectively the trieline product has colourity preferably, avoided the corrosion of carbon steel material to the pollution of product.
The rectifying section of tetrachloroethane tower, the rectifying section of desorption tower adopt the enamel material, and the low tower rectifying section that boils adopts fluorinated ethylene propylene (F40) tower joint.For improving the rectification effect of trieline tower, this tower is designed to valve tray column.For improving tower tray work-ing life, be stainless steel with float valve and tower tray material design.Resistance to corrosion and the rectification effect of each tower rectifying section like this, have greatly been improved.
Trieline and other intermediates are in the situation that there is oxygen to exist, and the generation organic acid that can react causes the rotten of product and consumes and rises.For avoiding trieline and other intermediates to contact with oxygen, nitrogen seal device is used in design on the test tank of intermediate tank farm and finished product tank field, storage tank, and the redundant space in container is occupied by nitrogen.Guarantee the quality of product, avoided the decomposition of trieline.
The raw material of producing trieline is chlorine and acetylene, and chlorine is hypertoxic medium, and acetylene chemistry character is active, and is inflammable and explosive.For further improving the security of producing, the present invention's device has been set a plurality of interlockings, be respectively the interlocking of acetylene compressor import and export pressure and compressor, the interlocking of compressor and chlorine, acetylene variable valve, the interlocking of tail water flow and chlorine, acetylene gas variable valve, the interlockings of chlorination tower vacuum tightness and chlorine, acetylene variable valve etc. have been guaranteed safety, the steady running of trieline device by above interlocking.
Chlorination tower moves under negative pressure state, and negative pressure is aspirated generation with hydraulic jet pump.In the process of suction, partial oxidation hydrogen, acetylene gas, chlorine and organic acid are dissolved in tail water, cause tail water acidity to be strengthened gradually.Other trielines producer when tail water acidity reaches certain numerical value, just replaces tail water, has not only polluted environment but also wasted water resources.The present invention's device is delivered to hydraulic jet pump with the tail water in afterbay with the tail water force (forcing) pump, chlorination tower is aspirated make it to produce negative pressure, and tail water, recycles to afterbay by the overflow of chlorination tail tank, has saved a large amount of water resourcess, has protected environment.
The trieline tower of other trielines producer adopts the discharging of trim the top of column liquid, product contains acid at 10-15ppm or higher, when being used as trieline and being metal cleaner and using, can erode metallic surfaces, the object that destruction is cleaned is to causing serious loss with trieline as the producer of clean-out system.On the present invention's device, the trieline tower is set up four side discharge ports, is located at respectively on the 5th, 7,9,11 layer of tower tray of rectifying section.The tower top discharging combines with the upper side discharge method, can effectively reduce trieline product acidity, and acidity can be controlled in below 5ppm.
Claims (4)
1 Trichloroethylene industrial production apparatus characterized in that it has an acetylene gas feed line and the inlet line with chlorine chlorination tower, (9) respectively connected to the inlet end, chlorination tower, (9) and the outlet end of the chlorination tower whole condenser, (7) is connected to the inlet end, the whole condenser chlorination tower, (7), respectively, with the outlet end of the reflux drum chloride, (8) the inlet end and the tail chlorination tower cooler, (6) is connected to the inlet end, chlorine the cold end of the rectification column, (6), respectively, the outlet end of the reflux drum chloride, (8) and the inlet end of the gas-liquid separator (5) connected to the inlet end of the gas-liquid separator (5) and the exhaust gas outlet end of the buffer tank, (4) import terminal is connected, the exhaust gas buffer tank, (4) with a water jet pump outlet end, (3) import terminal is connected, water jet pump, (3) the outlet end and tail chlorinated water tank (10) connected to the inlet end, Chloride tail water tank (1) inlet end (10) and the outlet end is connected to the pool tail chloride, chlorinated end of the pool, (a) the outlet end of the pressure pump (2) is connected to the inlet end, the pressure pump, (2 ) and the outlet end of the water jet pump (3) is connected to the inlet end of the other chloride, reflux tank, (8) and the outlet end of the rough tetrachloroethane tank (11) connected to the inlet end, the crude tetrachloroethane tank ( 11) and the outlet end of the column tetrachloroethane, (12) is connected to the inlet end, tetrachloroethane tower (12) and a lower outlet end, respectively, tetrachloroethane column reboiler (13) and the inlet end tetrachloride fine ethane tank (17) connected to the inlet end, tetrachloroethane column reboiler (13) and the outlet end of the column tetrachloroethane, (12) is connected to the inlet end of the other, tetrachloroethane tower (12 ) and the outlet end of the top full-tetrachloroethane tower condenser, (14) is connected to the inlet end, full-tetrachloroethane tower condenser, (14), respectively, with the outlet end tetrachloroethane tower reflux drum, (16) import terminal and tetrachloroethane tower cooler tail(15) is connected to the inlet end, tetrachloroethane column outlet end of the cold tail tetrachloroethane column reflux drum (16) is connected to the inlet end, tetrachloroethane finishing tank (17) and the outlet end of the vaporizer tetrachloroethane , (18) is connected to the inlet end, the outlet end of the vaporizer tetrachloroethane dehydrochlorination reactor feed preheater (21) connected to the inlet end, a dehydrochlorination reactor feed preheater (21) and the outlet end of the thermal oil preheater (19) connected to the inlet end, oil preheater (19) and the outlet end of the dehydrochlorination apparatus (20) is connected to the inlet end, a dehydrochlorination reaction means (20) and the outlet end of the dehydrochlorination reaction reactor feed preheater (21) connected to the inlet end of the other dehydrochlorination reactor feed preheater (21) and the other outlet end of the desorption column (22) is connected to the inlet end of the desorption column, (22) bottom of the outlet end of the desorption tower reboiler (23) is connected to the inlet end of the desorption column reboiler, (23) the outlet end and desorption tower (22) is connected to the other end of the import, export desorption tower at the top end and full desorption tower condenser, (24) import terminal connected, desorption tower full condensate outlet side, respectively desorption tower reflux drum, (26) import terminal and analytical column tail intercooler, (25) import terminal connected, analytic tower tail intercooler, (25) the outlet end of the desorption column reflux tank (26) connected to the inlet end of the desorption column reflux drum, (26) the outlet end of the reactor tank and analysis, (27) is connected to the inlet end, parsing tank reactor, (27) and the lower outlet end boiling tower (28) is connected to the inlet end, low-boiling column, (28) and a lower outlet end, respectively, the low-boiling column reboiler (29) and the inlet end of trichlorethylene tower (33) is connected to the inlet end of the low-boiling column reboiler outlet end of the inlet end of the low-boiling column is connected to the other, low-boiling column, (28) the top outlet end of the full low-boiling column condenser, (30) is connected to the inlet end, the whole low-boiling column condenser (30) outlet end respectively with low boiling tower reflux drum, (32) the inlet end and the low boiling tower tail intercooler, (31) import terminal is connected to the low boiling tower tail intercooler, (31) the outlet end and low-boiling tower reflux drum, (32) imports terminal connected, trichlorethylene column( 33 ) and a lower outlet end , respectively, trichlorethylene column reboiler ( 34 ) and the inlet end of the reactor tank of trichlorethylene and (39 ) is connected to the inlet end , trichlorethylene column reboiler ( 34 ) and the outlet end trichlorethylene tower ( 33 ) is connected to the inlet end of the other , trichlorethylene tower ( 33 ) and the upper outlet end of the whole column condenser trichlorethylene , ( 35 ) is connected to the inlet end , the whole column condenser trichlorethylene , ( 35 ) and the outlet end of each end of the cold tower trichlorethylene , ( 36 ) and the inlet end of trichlorethylene tower reflux tank ( 37 ) connected to the inlet end , the end of the cold tower trichlorethylene , ( 36 ) and the outlet end of the column trichlorethylene reflux tank ( 37 ) connected to the inlet end , a reflux column trichlorethylene tank ( 37 ) and the outlet end of each column trichlorethylene , ( 33 ) the inlet end of the other , the material cooler trichlorethylene , ( 38 ) the inlet end connected to the reactor tank trichlorethylene , ( 39 ) the outlet end of the column and the intermediate fraction , ( 40 ) is connected to the inlet end , a middle distillate tower ( 40 ) , respectively, the lower outlet end of the column and the intermediate reboiler fraction , ( 41 ) the inlet end and tetrachlorethylene towers, ( 45 ) is connected to the inlet end of the middle distillate tower, ( 40 ) the upper and middle distillate outlet end full tower condenser , ( 42 ) is connected to the inlet end of the middle distillate full tower condenser , ( 42 ) the outlet end respectively, and the middle distillate tower tail intercooler, ( 43 ) the inlet end and middle distillate tower reflux drum , ( 44 ) import terminal connected to the middle distillate tower tail intercooler, ( 43 ) the outlet end and middle distillates tower reflux drum , ( 44 ) other inlet end connected to the intermediate tank ends column reflux , ( 44 ) and the outlet end of the desorption column bottom liquid tank ( 27 ) connected to the inlet end of the other , tetrachlorethylene column(45) with the lower outlet end of the column reboiler tetrachlorethylene, (46) inlet end, tetrachlorethylene column (45) and the upper outlet end of the condenser tetrachlorethylene whole column, (47) is connected to the inlet end, tetrachlorethylene full tower condenser, (47), respectively, with the outlet end of tetrachlorethylene tower reflux drum, (49) and tetrachlorethylene import terminal tail intercooler, (48) is connected to the inlet end, tetrachlorethylene tail intercooler, (48) exports Tetrachloroethylene end tower reflux tank (49) connected to the inlet end of the other, the whole of the condenser, the cold end of the heat exchanger device is used for each piece of graphite impregnated phenolic resin.
2. industrial production apparatus for trichloroethylene as claimed in claim 1, it is characterized in that, described acetylene admission line is connected with chlorination tower (9) entrance end through acetylene gas drying purification device (50), there is acetylene admission line (523) to be connected with acetylene compressor (51) entrance end on acetylene gas drying purification device (50), acetylene compressor (51) exit end is connected with acetylene water cooler (52) entrance end, acetylene cooler outlet end is connected with acetylene spray catcher (53) entrance end, acetylene spray catcher top exit end is connected with dry I tower (56) the lower inlet end of sulfuric acid, the dry I tower of sulfuric acid top exit end is connected with dry II tower (59) the lower inlet end of sulfuric acid, the dry II tower of sulfuric acid top exit end is connected with dry III tower (512) the lower inlet end of sulfuric acid, the dry III tower of sulfuric acid top exit end is connected with acetylene acid separator (515) entrance end, acetylene acid separator top exit end is connected with acetylene adsorption tower (517) entrance end, another exit end of acetylene water cooler (52) is connected with moisture holding tank (54) entrance end, acetylene spray catcher (53) lower part outlet end is connected with moisture holding tank (54) entrance end, vitriol oil storage tank (520) exit end is connected with vitriol oil transferpump (522) entrance end, vitriol oil transferpump exit end is connected with concentrated sulfuric acid cooler (514) entrance end, the concentrated sulfuric acid cooler exit end is connected with dry III tower (512) the upper inlet end of sulfuric acid, dry III tower (512) the lower part outlet end of sulfuric acid is connected with dry II tower (59) the lower inlet end of sulfuric acid, dry another lower part outlet end of III tower (512) of sulfuric acid is connected with dry III tower sulfuric acid recycle pump (513) entrance end of sulfuric acid, dry III tower sulfuric acid recycle pump (513) exit end of sulfuric acid is connected with dilute sulphuric acid recirculation cooler (511) entrance end, dilute sulphuric acid recirculation cooler (511) exit end is connected with dry III tower (512) the upper inlet end of sulfuric acid, dry II tower (59) the lower part outlet end of sulfuric acid is connected with dry I tower (56) the lower inlet end of sulfuric acid, dry another lower part outlet end of II tower (59) of sulfuric acid is connected with dry II tower sulfuric acid recycle pump (510) entrance end of sulfuric acid, dry II tower sulfuric acid recycle pump (510) exit end of sulfuric acid is connected with another dilute sulphuric acid recirculation cooler (58) entrance end, another dilute sulphuric acid recirculation cooler (58) exit end is connected with dry II tower (59) the upper inlet end of sulfuric acid, dry I tower (56) the lower part outlet end of sulfuric acid is connected with dry I tower sulfuric acid recycle pump (57) entrance end of sulfuric acid, dry I tower sulfuric acid recycle pump (57) exit end of sulfuric acid is connected with the 3rd dilute sulphuric acid recirculation cooler (55) entrance end, the 3rd dilute sulphuric acid recirculation cooler (55) exit end is connected with dry I tower (56) the upper inlet end of sulfuric acid, dry another lower part outlet end of I tower (56) of sulfuric acid is connected with dilute sulphuric acid storage tank (519), nitrogen buffer tank (521) is connected with acetylene adsorption tower (517) lower inlet end through nitrogen electric heater (518).
3. industrial production apparatus for trichloroethylene as claimed in claim 1 or 2, it is characterized in that, on described dehydrochlorination reaction device (20), at least 3 tetrachloroethane vaporizers (202) are arranged, also have the quantity dehydrochlorination reaction device (206) identical with the tetrachloroethane vaporizer, the import of each tetrachloroethane vaporizer is connected with feeding line (201) through valve respectively, the outlet of each tetrachloroethane vaporizer is connected through the import of valve with the dehydrochlorination reaction device respectively, the outlet of each dehydrochlorination reaction device is connected with discharging pipeline (209) through valve respectively, between the outlet of each dehydrochlorination reaction device also through valve, pipeline (208) is connected, between the import of each dehydrochlorination reaction device also through valve, another pipeline (205) is connected, pipeline, be connected by connection line (207) between another pipeline, the outlet of each tetrachloroethane vaporizer is also through valve, the 3rd pipeline (203) is connected.
4. industrial production apparatus for trichloroethylene as claimed in claim 1 or 2, it is characterized in that, on gas distributor in described chlorination tower (9), main distribution pipe (91) is arranged, main distribution pipe two ends are horizontally connected with short distribution pipe (92), the middle part is horizontally connected with the distribution pipe of drawing money on credit (94), short distribution pipe, draw money on credit have between distribution pipe in distribution pipe (93) cross connection on main distribution pipe, vertical direction at main second circumference of distribution pipe tube wall, the vertical direction both sides have respectively one to discharge pore (101), be distributed with many row's distribution pipe production wells (301) on second circumference of each distribution pipe tube wall.
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| CN102775269A (en) * | 2012-07-13 | 2012-11-14 | 中国石油集团东北炼化工程有限公司葫芦岛设计院 | Trichloroethylene gas phase catalysis production method |
| CN103467240B (en) * | 2013-09-23 | 2015-04-08 | 芜湖融汇化工有限公司 | System for separating hydrogen chloride in coarse trichloroethylene |
| CN108438579A (en) * | 2018-03-23 | 2018-08-24 | 江苏安邦电化有限公司 | A kind of N-butyl raw material finished product storage tank nitrogen seal device |
| CN110479124A (en) * | 2019-08-09 | 2019-11-22 | 浙江衢州巨塑化工有限公司 | A kind of tetrachloroethanes process units and its method |
| CN111087280B (en) * | 2020-01-22 | 2023-08-29 | 辽宁方大工程设计有限公司 | Production method for preparing trichloroethylene by acetylene chlorination-gas phase catalytic dehydrochlorination |
| CN114272885A (en) * | 2021-12-28 | 2022-04-05 | 厦门中科易工化学科技有限公司 | Tower reactor for synthesizing chloroethylene and application thereof |
| CN114455221A (en) * | 2022-03-14 | 2022-05-10 | 滨化集团股份有限公司 | System and method for controlling tank top pressure of normal-pressure storage tank with nitrogen seal |
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| CN101353289A (en) * | 2008-08-19 | 2009-01-28 | 何勇志 | Method for extracting trans-dichloroethylene from low-boiling residue of ethinyltrichloride production by gas-phase catalytic process |
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| CN201762266U (en) * | 2010-06-01 | 2011-03-16 | 滨化集团股份有限公司 | Trichloroethylene industrialized production device |
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| FR2910350B1 (en) * | 2006-12-22 | 2009-01-30 | Solvay | CATALYTIC HYDROCHLORIZATION SYSTEM AND PROCESS FOR PRODUCING VINYL CHLORIDE FROM ACETYLENE AND HYDROGEN CHLORIDE IN THE PRESENCE OF THIS CATALYTIC SYSTEM |
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| CN101353289A (en) * | 2008-08-19 | 2009-01-28 | 何勇志 | Method for extracting trans-dichloroethylene from low-boiling residue of ethinyltrichloride production by gas-phase catalytic process |
| CN101514140A (en) * | 2009-04-02 | 2009-08-26 | 成都惠恩精细化工有限责任公司 | Method for preparing vinyl chloride by hydrochlorination of acetylene |
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Denomination of invention: Industrial production apparatus for trichloroethylene Effective date of registration: 20190102 Granted publication date: 20130619 Pledgee: Binzhou Bincheng Branch of China Construction Bank Co., Ltd. Pledgor: Befar Group Co.,Ltd. Registration number: 2018370000240 |
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