CN101912718B - Device and method for absorbing carbon disulfide in hydrogen sulfide gas by using solvent - Google Patents
Device and method for absorbing carbon disulfide in hydrogen sulfide gas by using solvent Download PDFInfo
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- CN101912718B CN101912718B CN201010257621XA CN201010257621A CN101912718B CN 101912718 B CN101912718 B CN 101912718B CN 201010257621X A CN201010257621X A CN 201010257621XA CN 201010257621 A CN201010257621 A CN 201010257621A CN 101912718 B CN101912718 B CN 101912718B
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Abstract
The invention discloses a device and a method for absorbing carbon disulfide in hydrogen sulfide gas by using solvent, which belong to the technical field of hydrogen sulfide gas and carbon disulfide preparation. The device of the invention mainly comprises an absorption tower, an analytical tower, a gas-liquid separator, a heat exchanger, a cooler, a heater, a pump, a valve and the like; and the method is to produce H2S and CS2 products by using the device and absorption and separation in a transfer mass dynamic control process and solvent. The device of the invention has a simple structure and low cost; and the method of the invention has the advantages of good absorption/separation effect, full utilization of resources, reduced energy consumption, low production cost and convenient popularization and application, wherein the absorption rate of CS2 is up to 99 percent. The device and the method of the invention can be widely applied to separation of H2S gases and CS2 in industrial production, particularly the separation of CS2 from H2S gases in the process of preparing CS2 by using natural gases.
Description
Technical field
The invention belongs to the technical field that removes carbon disulfide in the hydrogen sulfide gas, be specifically related to utilize natural gas to prepare in the hydrogen sulfide gas process, from hydrogen sulfide gas, separate the device and method of carbon disulfide.
Background technology
Hydrogen sulfide gas is generally as the natural decomposition product of chemical reaction or protein and be present in the multiple production process and occurring in nature, and wherein, being used for the synthetic of methionine is one of its purposes.Industry is at present gone up the production methionine and is generally adopted methylthiopropionaldehyde condensation water solution, promptly generates methylthiopropionaldehyde with methyl mercaptan and acrolein reaction, and methylthiopropionaldehyde carries out the condensation hydrolysis again and makes methionine.And methyl mercaptan often by methyl alcohol and hydrogen sulfide gas at molybdic acid/Al
2O
3The effect of catalyst is synthetic down.At present; The preparation method commonly used of hydrogen sulfide gas is by methane and elemental sulfur preparation; Methane and elemental sulfur reaction obtain carbon disulfide and hydrogen sulfide mixture; Obtain hydrogen sulfide gas and by-product carbon disulfide after separate, but existing technology, especially low-pressure process technology can't be removed the carbon disulfide in the hydrogen sulfide gas fully.Can synthesize the molybdic acid catalyst by the follow-up methyl mercaptan of appreciable impact and contain a spot of carbon disulfide in the hydrogen sulfide, cause catalyst activity to reduce and the lost of life.In addition, above-mentioned hydrogen sulfide preparation technology also is that the common method of producing carbon disulfide is gone up in industry, faces the problem of a small amount of carbon disulfide in the hydrogen sulfide gas in this technology equally.Therefore seek the new method of a small amount of carbon disulfide in the new Separation and Recovery hydrogen sulfide gas, commercial production hydrogen sulfide gas or carbon disulfide are had important economy and technical meaning.
The existing device and method that reclaims a small amount of carbon disulfide in the hydrogen sulfide gas; Like application number is " reclaiming the Apparatus and method for of carbon disulfide in the hydrogen sulfide gas in the carbon disulphide manufacture " patent of 200610127381.5, and disclosed equipment mainly comprises: the adsorptive reactor of dress adsorbent in 2～4 or more, adsorption-buffering jar, in the complicated apparatus such as absorption preprocessor, vacuum analysis pump, surge tank and appendix, vacuum tube, valve of sulphur adsorbent are housed.Disclosed method is to utilize this device to carry out transformation absorption; Be about to adsorb the hydrogen sulfide gas that contains carbon disulfide that preprocessor is separated; Under system pressure and condition, send at least two adsorptive reactors near absorption preprocessor tip temperature; The absorption of the transformation that hockets respectively, vacuum desorption operation, the hydrogen sulfide gas after the absorption drains into Crouse's recovery system, and the carbon disulfide mist after the desorb gets into refined unit and reclaims carbon disulfide.The major defect of this method is: complex equipments, and the production cycle is long, and energy consumption is high, and cost is high, and the scope of application is little, and inconvenience is applied, and more is not suitable for suitability for industrialized production.
Summary of the invention
The objective of the invention is the weak point to carbon disulfide device and method in the existing separate hydrogen sulfide gas, a kind of device and method with carbon disulfide in the solvent absorbing hydrogen sulphide gas is provided, it is simple to have a device structure; Method is simple; Cost is low, conservation and energy, and environmental pollution is little; Applied widely, be convenient to characteristics such as commercial production.
Mechanism of the present invention: contain carbon disulfide (CS
2) hydrogen sulfide (H
2S) gaseous mixture gets into the absorption tower at normal temperatures at the bottom of the tower, and from the cat head spray and solvent adverse current down fully contacts, because the solvent and the CS of selection
2Can infinitely dissolve each other, and not dissolve H basically
2S, so CS
2Can be to greatest extent and H
2S separates.Because this process is the mass transfer dynamics control procedure,, absorbed CS again for reaching purpose of energy saving
2The absorption rich solution can partly recycle use.After another part absorbs rich solution and carries out heat exchange from the next high temperature regeneration liquid of Analytic Tower, get into Analytic Tower, heating is to remove CS
2Afterwards obtain regeneration.The high temperature regeneration lean solution of coming out from Analytic Tower after carrying out heat exchange and recycle heat with the low temperature rich solution that comes from the absorption tower, came back to the absorption tower before getting into the absorption tower.The CS that the Analytic Tower top obtains
2Through condensation and gas-liquid separation, reclaim CS
2, and the H on gas-liquid separator top
2S and CS
2Gaseous mixture is returned absorber and is carried out absorption and separation.
Realize that the object of the invention technical scheme is: a kind ofly absorb H with solvent
2CS in the S gas
2Device, mainly comprise absorption tower, Analytic Tower, the 1st gas-liquid separator and the 2nd gas-liquid separator, heat exchanger, cooler, heater, pump and valve etc.
Described absorption tower for down thick thin upper and lower two sections to improve absorption efficiency and to save energy.Bottom one side at the hypomere on absorption tower is provided with a through hole, and 1st flow control valve, 1st three-way pipe and the tube connector of this through hole through the band flowmeter (promptly contains a small amount of CS with the inner chamber and the mixed raw material gas of absorption tower hypomere
2H
2The S gaseous mixture) generation device is communicated with.Mixed raw material gas gets into the bottom on absorption tower through tube connector through the straight tube of the 1st flow control valve and the 1st three-way pipe of band flowmeter, in the absorption tower, flows from bottom to top.Bottom centre place on the absorption tower is provided with a through hole, and this through hole is communicated with the import of booster pump through the straight tube and the tube connector of the 2nd three-way pipe, and the arm of the 2nd three-way pipe is communicated with inlet of circulating pump through tube connector.Outlet of circulating pump is communicated with the through hole that hypomere top, absorption tower one side is provided with through the 2nd flow control valve and the tube connector of band flowmeter; Be positioned over the part of the solvent of absorption tower hypomere through hole; Under the effect of circulating pump,, in the hypomere on absorption tower,, liquid distribution trough flows from the top down after disperseing through the top of this through hole entering absorption tower hypomere; Fully contact with the mixed raw material gas that flows from bottom to top, absorb the CS in the mixed raw material gas
2, remove CS in the mixed raw material gas in order to reach
2Purpose.The supercharging delivery side of pump is communicated with the interior pipe import of heat exchanger through the 3rd flow control valve and tube connector, and the outlet of the interior pipe of heat exchanger is communicated with the through hole that Analytic Tower top one side is provided with through tube connector, is absorbed with CS
2Solvent (abbreviation rich solution) through the heat exchanger preheating after this through hole gets into the top of Analytic Tower epimere, after liquid distribution trough disperses, in Analytic Tower, flow from top to bottom and emit CS
2And regenerate.Top one side of epimere is provided with a through hole on the absorption tower; The top that solvent after the Analytic Tower regeneration and the solvent after the 1st gas-liquid separator separates get into the absorption tower; And in the absorption tower, flow from the top down, with the gas that flows from bottom to top (CS in the mist of the epimere on absorption tower
2The hypomere gas on concentration ratio absorption tower in CS
2Concentration low) fully contact, absorb the CS in the mist
2, further to remove the CS in the gaseous mixture
2Center, top on the absorption tower is provided with a through hole, and this through hole is communicated with the through hole that the 1st gas-liquid separator one side is provided with through tube connector, removes CS in the absorption tower
2The through hole of hydrogen sulfide gas through the top, absorption tower get into the 1st gas-liquid separator; In the 1st gas-liquid separator, carry out gas-liquid separation; The through hole that liquid after the separation (being solvent) is provided with through the 1st gas-liquid separator bottom centre place by the arm of the 4th flow control valve of band liquid level gauge and tube connector and the 3rd three-way pipe with mix from the next regenerated solvent of Analytic Tower after the top of entering absorption tower epimere, get back to and absorb CS in the absorption tower again
2Gas after the separation (promptly removes CS
2Purification H
2S gas) through hole that is provided with through the 1st gas-liquid separator top center place and tube connector are collected.
Described Analytic Tower is divided into upper and lower two sections, resolves effect and saves energy in order to the resolution temperature and the raising of solvent in the control tower.The rich solution that transports through booster pump from the absorption tower (promptly is absorbed with CS
2Solvent) temperature raises behind heat exchanger, the through hole through Analytic Tower epimere one side gets into Analytic Tower again, and after liquid distribution trough disperses, in Analytic Tower, flows from top to bottom.On Analytic Tower top, rich solution (promptly is absorbed with CS
2Solvent) in CS
2Part takes place resolves.The homonymy on pars infrasegmentalis one side and hypomere top on Analytic Tower; One through hole is set respectively; This two through hole is communicated with the two ends of pipe in the heater through tube connector respectively, in heater, is provided with thermocouple thermometer on the tube connector of pipe outlet simultaneously, to measure the temperature of solvent.Heater is the CS that comes from the Analytic Tower epimere
2The rich solution of part parsing (promptly is absorbed with CS
2Solvent) heat is provided, further improve the temperature of rich solution.Rich solution after the heating is back in the Analytic Tower through the through hole on Analytic Tower hypomere top, after liquid distribution trough disperses, at the mobile from top to bottom one-step removal CS that goes forward side by side of Analytic Tower hypomere
2Resolve to lean solution and (promptly isolate CS
2Solvent).The through hole on pipe, epimere top, absorption tower in the 5th flow control valve of the through hole that the lean solution after Analytic Tower is resolved is provided with through Analytic Tower bottom centre place, tube connector, band liquid level gauge, the heat exchanger gets into the absorption tower in order to absorb the CS in the gas in the absorption tower
2CS after Analytic Tower is resolved
2The demister that at first is provided with at the Analytic Tower inner top is removed entrained liquid (being solvent); The through hole and the tube connector that are provided with through Analytic Tower top center place then communicate with the interior pipe import of cooler, and the outlet of pipe is communicated with the through hole that a side of the 2nd gas-liquid separator is provided with through tube connector in the cooler.In cooler, most of CS
2Gas is cooled into liquid, and thermocouple thermometer is set to show CS on the tube connector of cooler outlet
2Temperature after gas is cooled.In the 2nd gas-liquid separator, cooled CS
2Liquid with contain small amount of H
2The CS of S
2Gas carries out gas-liquid separation, and the gas after the separation (promptly contains H
2The CS of S
2Gas) through hole that is provided with through the 2nd gas-liquid separator top center place, tube connector, (promptly contain a small amount of CS with the arm and the mixed raw material gas of manometric the 6th flow control valve, the 1st three-way pipe
2H
2The S mist) mixes the back and get into the absorption tower hypomere; The CS that the 2nd gas-liquid separator separates goes out
2Liquid, the 7th flow control valve of through hole that is provided with through the 2nd gas-liquid separator bottom centre place and tube connector and band liquid level gauge is collected.
Described heat exchanger is conventional tubular heat exchanger.In heat exchanger, the rich solution after the booster pump supercharging (promptly is absorbed with CS
2Solvent) in managing, flow through, the lean solution after Analytic Tower is resolved (promptly removes CS
2Solvent) outside managing, flow through, lean solution and rich solution carry out heat exchange, and rich solution is carried out preheating, make full use of heat energy, reduce energy consumption.
Described heater is conventional shell and tube steam heater, and heat medium is the low pressure (steam of 1.4MPa >=P >=0.7MPa).
Described cooler is conventional shell and tube water cooler, and cooling medium is a water.
A kind of method with carbon disulfide in the solvent absorbing hydrogen sulphide is utilized apparatus of the present invention, adsorbs, separates and get H through solvent and mass transfer dynamics principle control procedure
2S and CS
2Product.Its concrete step is following:
(1) absorbs
With CS
2Initial concentration be 10%, pressure is that the mixed raw material gas of 0.2～0.4MPa (is H
2Contain a small amount of CS in the S gas
2Mist), the input of bottom one side through hole of hypomere is flowed in the absorption tower from bottom to top from the absorption tower.The solvent (being paraffin oil or machine oil or No. 200 solvent equal solvents) that is positioned over the absorption tower is forced into 0.25～0.45MPa through circulating pump, and the through hole of the hypomere top one side input from the absorption tower behind liquid distribution trough, sprays in the hypomere on absorption tower from the top down.And (be absorbed with CS from the circulation lean solution of Analytic Tower bottom
2Paraffin oil or machine oil or No. 200 solvent equal solvents), the through hole of top one side of the epimere input from the absorption tower, through behind the liquid distribution trough in the absorption tower spray from the top down, fully contact with the mixed raw material gas that flows from bottom to top and absorb CS
2Solvent: the mass ratio of mixed raw material gas is 1: 0.72～2.8.
(2) resolve
After the completion of (1) step, (1) step of warp in the absorption tower is absorbed with CS
2The part of solvent (abbreviation rich solution), be pressurized to 0.3～0.5MPa through booster pump earlier, after heat exchanger carries out preheating; Be preheated to 110～130 ℃; Get into the epimere of Analytic Tower then through tube connector, flow from top to bottom in tower through liquid distribution trough, after resolving; Be heated to 120～140 ℃ through heater again, further fully resolve and become lean solution at the hypomere of Analytic Tower and (promptly remove CS
2Solvent), last lean solution is delivered to heat exchanger from the bottom through-hole output of Analytic Tower and through tube connector, is cooled to 30～35 ℃ through the heat exchanger heat exchange, gets in the absorption tower through the through hole of epimere top, absorption tower one side through tube connector and is used further to absorb CS
2
(3) gas-liquid separation
(1) step in the absorption tower, absorbed CS through (1) step solvent after accomplishing
2H
2S gas, through hole and tube connector through the top, absorption tower are imported the 1st gas-liquid separator and are carried out gas-liquid separation, and the gas after the separation (is the H of purification
2S gas) be finished product, collect through the through hole and the tube connector output at the 1st gas-liquid separator top; Liquid after the separation (being solvent) through the through hole of the 1st gas-liquid separator bottom and the through hole of tube connector and epimere top, absorption tower one side, gets in the absorption tower and is used further to absorb CS
2
In Analytic Tower, the gas after (2) step resolved (promptly is absorbed with CS
2Gas) deliver in the cooler pipe through the through hole at Analytic Tower top and tube connector and be cooled to 5～10 ℃ and become gas-liquid mixture, get into the 2nd gas-liquid separator from the 2nd gas-liquid separator one side through hole and carry out gas-liquid separation, the liquid after the separation (is CS
2Liquid) be finished product, collect through the bottom through-hole and the tube connector output of the 2nd gas-liquid separator; Gas to after separating (promptly contains small amount of H
2The CS of S
2Gas) through the through hole at the 2nd gas-liquid separator top, tube connector, (promptly contain a small amount of CS with the arm and the mixed raw material gas of manometric the 6th flow control valve and the 1st three-way pipe
2H
2The S mist) after the mixing,, gets into the absorption tower recycling through the through hole of one side of pars infrasegmentalis under the absorption tower.
After the present invention adopts technique scheme, mainly contain following effect:
(1) absorption and separation is effective.To H after the absorption and separation of the present invention
2CS in the gas of S
2Carry out chromatography, its concentration drops to 0.1%～0.8% by initial 10%, can be used for the reaction of follow-up synthesis of methyl mercaptan, and very little to the influence of catalyst.Therefore, absorption and separation of the present invention is effective.
(2) CS
2Absorptivity is high.The approximately high-absorbility of the present invention can reach 99%.
(3) help environmental protection.CS
2Can recycle after the condensation at process Analytic Tower top and the gas-liquid separation, this had both made full use of resource, helped environmental protection again, and had reduced production cost.
(4) economize in raw materials and energy.Absorbed CS
2Absorption liquid can the part directly recycle, increased gas-liquid contact time; The H on the 2nd gas-liquid separator top
2S and CS
2Gaseous mixture come back to absorber, can realize the closed cycle of whole process, realize zero-emission.The regeneration lean solution before getting into the absorption tower, with the rich solution heat exchange that comes from the absorption tower, making full use of heat, energy savings, thus further cut down the consumption of energy and production cost.
(5) apparatus of the present invention are simple in structure, and operation is simple, and machine utilization is big, invest for a short time, and cost is low, and is easy to utilize.
The present invention can be widely used in Separation and Recovery H in the commercial production
2A small amount of CS in the S gas
2, can prepare highly purified H
2S gas and CS
2, be specially adapted to prepare CS with natural gas
2In the process, from H
2Separation of C S in the S gas
2
Description of drawings
Fig. 1 is the structural representation of apparatus of the present invention.
Among the figure: 1-absorption tower, 2-Analytic Tower, 3-the 1st gas-liquid separator, 4-the 2nd gas-liquid separator, 5-heat exchanger, 6-cooler, 7-heater, 8-circulating pump, 9-booster pump, F-flowmeter, L-liquid level gauge, P-Pressure gauge, T-thermometer.
The specific embodiment
Below in conjunction with the specific embodiment, further specify the present invention.
Embodiment 1
As shown in Figure 1, a kind of device with carbon disulfide in the solvent absorbing hydrogen sulphide gas mainly comprises absorption tower 1, Analytic Tower the 2, the 1st gas-liquid separator 3 and the 2nd gas-liquid separator 4, heat exchanger 5, cooler 6, heater 7, pump 8,9 and valve etc.
Described absorption tower 1 for down thick thin upper and lower two sections to improve absorption efficiency and to save energy.Bottom one side of 1 hypomere is provided with a through hole on the absorption tower, and this through hole is communicated with the inner chamber of absorption tower 1 hypomere through the 1st flow control valve, the 1st three-way pipe and the tube connector of band flowmeter with the mixed raw material gas generation device.Mixed raw material gas gets into the bottom on absorption tower 1 through tube connector through the straight tube of the 1st flow control valve and the 1st three-way pipe of band flowmeter, in absorption tower 1, flows from bottom to top.1 bottom centre place is provided with a through hole on the absorption tower, and this through hole is communicated with the import of booster pump 9 through the straight tube and the tube connector of the 2nd three-way pipe, and the arm of the 2nd three-way pipe is communicated with through the import of tube connector with circulating pump 8.The outlet of circulating pump 8 is communicated with the through hole that 1 hypomere top, absorption tower, one side is provided with through the 2nd flow control valve and the tube connector of band flowmeter; Be positioned over the part of the solvent of absorption tower 1 hypomere through hole; Under the effect of circulating pump 8,, in the hypomere on absorption tower 1,, liquid distribution trough flows from the top down after disperseing through the top of this through hole entering absorption tower 1 hypomere; Fully contact with the mixed raw material gas that flows from bottom to top, absorb the CS in the mixed raw material gas
2, remove CS in the mixed raw material gas in order to reach
2Purpose.The outlet of booster pump 9 is communicated with the interior pipe import of heat exchanger 5 through the 3rd flow control valve and tube connector, and the outlet of the interior pipe of heat exchanger 5 is communicated with the through hole that Analytic Tower 2 tops one side is provided with through tube connector, is absorbed with CS
2Solvent through heat exchanger 5 preheatings after this through hole gets into the top of Analytic Tower 2 epimeres, after liquid distribution trough disperses, in Analytic Tower 2, flow from top to bottom and emit CS
2And regenerate.Top one side of 1 epimere is provided with a through hole on the absorption tower; The top on solvent after Analytic Tower 2 regeneration and solvent entering absorption tower 1 after the 1st gas-liquid separator 3 separates; And in absorption tower 1, flow from the top down, fully contact with the gas that flows from bottom to top, absorb the CS in the gaseous mixture
2, further to remove the CS in the gaseous mixture
21 center, top is provided with a through hole on the absorption tower, and this through hole is communicated with the through hole that the 1st gas-liquid separator 3 one sides are provided with through tube connector, removes CS in the absorption tower 1
2H
2One through hole on S gas 1 top through the absorption tower gets into the 1st gas-liquid separator 3; In the 1st gas-liquid separator 3, carry out gas-liquid separation; The through hole that liquid after the separation is provided with through the 1st gas-liquid separator 3 bottom centre places is by the top of the arm of the 4th flow control valve of band liquid level gauge and tube connector and the 3rd three-way pipe with entering absorption tower 1 epimere after regenerated solvent from Analytic Tower 2 mixes, and gets back to absorb CS in the absorption tower 1 again
2Through hole and tube connector that gas after the separation is provided with through the 1st gas-liquid separator 3 top center places are collected.
Described Analytic Tower 2 is divided into upper and lower two sections, resolves effect and saves energy in order to the resolution temperature and the raising of solvent in the control tower.1 rich solution temperature behind heat exchanger of transporting through booster pump 9 raises from the absorption tower, and the through hole through Analytic Tower 2 epimeres one side gets into Analytic Tower 2 again, and after liquid distribution trough disperses, in Analytic Tower 2, flows from top to bottom.At Analytic Tower 2 tops, CS in the rich solution
2Part takes place resolves.The homonymy on pars infrasegmentalis one side and hypomere top on Analytic Tower 2; One through hole is set respectively; This two through hole is communicated with the two ends of pipe in the heater 7 through tube connector respectively, in heater 7, is provided with thermocouple thermometer on the tube connector of pipe outlet simultaneously, to measure the temperature of solvent.Heater 7 is the CS that comes from Analytic Tower 2 epimeres
2The rich solution of part parsing provides heat, further improves the temperature of rich solution.The through hole of rich solution after the heating through Analytic Tower 2 hypomere tops is back in the Analytic Tower 2, after liquid distribution trough disperses, at the mobile from top to bottom one-step removal CS that goes forward side by side of Analytic Tower 2 hypomeres
2Resolve to lean solution.The through hole on pipe, 1 epimere top, absorption tower in the 5th flow control valve of the through hole that the lean solution after Analytic Tower 2 is resolved is provided with through Analytic Tower 2 bottom centre place, tube connector, band liquid level gauge, the heat exchanger 5 gets into absorption tower 1 in order to absorb the CS in the gas in the absorption tower 1
2CS after Analytic Tower 2 is resolved
2The demister that at first is provided with at Analytic Tower 2 inner tops is removed entrained liquid; The through hole and the tube connector that are provided with through Analytic Tower 2 top center places then communicate with the interior pipe import of cooler 6, and the outlet of pipe is communicated with the through hole that a side of the 2nd gas-liquid separator 4 is provided with through tube connector in the cooler 6.In cooler 6, most of CS
2Gas is cooled into liquid, and thermocouple thermometer is set to show CS on the tube connector of cooler 6 outlets
2Temperature after gas is cooled.In the 2nd gas-liquid separator 4, cooled CS
2Liquid with contain small amount of H
2The CS of S
2Gas carries out gas-liquid separation, the through hole that the gas after the separation is provided with through the 2nd gas-liquid separator 4 top center places, tube connector, with the arm of manometric the 6th flow control valve, the 1st three-way pipe and entering absorption tower 1 hypomere after mixed raw material gas mixes; The 2nd gas-liquid separator 4 isolated CS
2Liquid, the 7th flow control valve of through hole that is provided with through the 2nd gas-liquid separator 4 bottom centre place and tube connector and band liquid level gauge is collected.
Described heat exchanger 5 is conventional tubular heat exchanger.In heat exchanger 5, the rich solution after booster pump 9 superchargings flows through in managing, and the lean solution after Analytic Tower 2 is resolved flows through outside managing, and lean solution and rich solution carry out heat exchange, and rich solution is carried out preheating, make full use of heat energy, reduce energy consumption.
Described heater 7 is conventional shell and tube steam heater, and heat medium is the low pressure (steam of 1.4MPa >=P >=0.7MPa).
Described cooler 6 is conventional shell and tube water cooler, and cooling medium is a water.
Embodiment 2
A kind of concrete steps with the method for carbon disulfide in the solvent absorbing hydrogen sulphide are following:
(1) absorbs
With CS
2Initial concentration be 10%, pressure is the mixed raw material gas of 0.3MPa, the input of bottom one side through hole of 1 hypomere is flowed in absorption tower 1 from bottom to top from the absorption tower.The paraffin oil solvent that is positioned over Analytic Tower 2 is forced into 0.35MPa through circulating pump 8, and the through hole of 1 hypomere top, the one side input from the absorption tower behind liquid distribution trough, sprays in the hypomere on absorption tower 1 from the top down.And from the circulation lean solution of Analytic Tower 2 bottoms, the through hole of top one side of the 1 epimere input from the absorption tower, through behind the liquid distribution trough in absorption tower 1 spray from the top down, fully contact with the mixed raw material gas that flows from bottom to top and absorb CS
2The paraffin oil solvent: the mass ratio of mixed raw material gas is 1: 1.5.
(2) resolve
After the completion of (1) step, (1) step of warp in the absorption tower 1 is absorbed with CS
2The part of solvent, be pressurized to 0.4MPa through booster pump 9 earlier, after heat exchanger 5 carries out preheating; Be preheated to 120 ℃, get into the epimere of Analytic Tower 2 then through tube connector, in tower, flow from top to bottom through liquid distribution trough; After resolving; Be heated to 130 ℃ through heater 7 again, further fully resolve and become lean solution at the hypomere of Analytic Tower 2, last lean solution is delivered to heat exchanger 5 from the bottom through-hole output of Analytic Tower 2 and through tube connector; Be cooled to 35 ℃ through heat exchanger 5 heat exchange, in the through hole entering absorption tower 1 of 1 epimere top, absorption tower, one side, be used further to absorb CS through tube connector again
2
(3) gas-liquid separation
(1) step in absorption tower 1, absorbed CS through (1) step solvent after accomplishing
2H
2S gas, the through hole at 1 top and tube connector through the absorption tower are imported the 1st gas-liquid separator 3 and are carried out gas-liquid separation, and the gas after the separation is finished product, collects through the through hole and the tube connector output at the 1st gas-liquid separator 3 tops; Liquid after the separation through the through hole of the 1st gas-liquid separator 3 bottoms and the through hole of tube connector and 1 epimere top, absorption tower, one side, gets in the absorption tower 1 and is used further to absorb CS
2
In Analytic Tower 2; Gas after (2) step resolved is delivered to manage in the cooler 6 through the through hole at Analytic Tower 2 tops and tube connector and is cooled to 10 ℃ and becomes gas-liquid mixture; Get into the 2nd gas-liquid separator 4 from the 2nd gas-liquid separator 4 one side through hole and carry out gas-liquid separation; Liquid after the separation is finished product, collects through the bottom through-hole and the tube connector output of the 2nd gas-liquid separator 4; To the gas after separating through the arm of through hole, tube connector, the 6th flow control valve and the 1st three-way pipe at the 2nd gas-liquid separator 4 tops with after mixed raw material gas mixes, through the through hole of 1 time pars infrasegmentalis one side in absorption tower, entering absorption tower 1 recycling.
Embodiment 3
A kind of concrete steps with the method for carbon disulfide in the solvent absorbing hydrogen sulphide, with embodiment 2, wherein:
In (1) step, the paraffin oil solvent: the mass ratio of mixed raw material gas is 1: 2.4.
In (2) step, lean solution is cooled to 33 ℃ through heat exchanger 5.
In (3) step, the gas after the parsing is cooled to 8 ℃ through cooler 6.
A kind of concrete steps with the method for carbon disulfide in the solvent absorbing hydrogen sulphide, with embodiment 2, wherein:
In (1) step, the paraffin oil solvent: the mass ratio of mixed raw material gas is 1: 2.8.
In (2) step, lean solution is cooled to 30 ℃ through heat exchanger 5.
In (3) step, the gas after the parsing is cooled to 5 ℃ through cooler 6.
Embodiment 5
A kind of concrete steps with the method for carbon disulfide in the solvent absorbing hydrogen sulphide, with embodiment 2, wherein:
In (1) step, the paraffin oil solvent: the mass ratio of mixed raw material gas is 1: 2.8.
In (2) step, solvent is that 130 ℃ and heater via 7 are heated to 140 ℃ through the temperature of heat exchanger 5 preheatings.
Embodiment 6
A kind of concrete steps with the method for carbon disulfide in the solvent absorbing hydrogen sulphide, with embodiment 2, wherein:
In (1) step, the pressure of mixed raw material gas is 0.2MPa, and circulating pump 8 is forced into 0.25MPa, the paraffin oil solvent: the mass ratio of mixed raw material gas is 1: 2.8.
In (2) step, booster pump 9 is pressurized to 0.3MPa, and solvent is that 110 ℃ and heater via are heated to 120 ℃ through the temperature of heat exchanger 5 preheatings.
Embodiment 7
A kind of concrete steps with the method for carbon disulfide in the solvent absorbing hydrogen sulphide, with embodiment 2, wherein:
In (1) step, the pressure of mixed raw material gas is 0.4MPa, and circulating pump 8 is forced into 0.45MPa, the paraffin oil solvent: the mass ratio of mixed raw material gas is 1: 2.8.
In (2) step, booster pump 9 is pressurized to 0.5MPa, and solvent is that 130 ℃ and heater via 7 are heated to 140 ℃ through the temperature of heat exchanger 5 preheatings.
Embodiment 8
A kind of concrete steps with the method for carbon disulfide in the solvent absorbing hydrogen sulphide, with embodiment 2, wherein:
In (1) step, the solvent that is used to absorb is a machine oil, the machine oil solvent: the mass ratio of mixed raw material gas is 1: 2.8.
Embodiment 9
A kind of concrete steps with the method for carbon disulfide in the solvent absorbing hydrogen sulphide, with embodiment 2, wherein:
In (1) step, the solvent that is used to absorb is No. 200 solvents, No. 200 solvents: the mass ratio of mixed raw material gas is 1: 2.8.
Experimental result
1, in the method to embodiment 2～4, under all identical condition of the heating-up temperature of the preheat temperature of the pressure of absorbent, mixed raw material gas pressure, circulating pump and booster pump, heat exchanger and heater, just liquid-gas ratio not simultaneously, to CS
2Absorptivity following: table 1
2, in the method to embodiment 4,5, under all identical condition of the pressure of absorbent, liquid-gas ratio, mixed raw material gas pressure, circulating pump and booster pump, just the heating-up temperature of the preheat temperature of heat exchanger and heater not simultaneously, to CS
2Absorptivity following: table 2
3, in the method to embodiment 4,6,7, under all identical condition of absorbent, liquid-gas ratio, and the heating-up temperature of the preheat temperature of the pressure of mixed raw material gas pressure, circulating pump and booster pump, heat exchanger and heater is not simultaneously, to CS
2Absorptivity following:
Table 3
4, in the method to embodiment 4,8,9, under all identical condition of the heating-up temperature of the preheat temperature of the pressure of liquid-gas ratio, mixed raw material gas pressure, circulating pump and booster pump, heat exchanger and heater, just lyosoption not simultaneously, to CS
2Absorptivity following:
Table 4
| Embodiment | Lyosoption | CS
2Absorb back | Absorptance | |
| 4 | Paraffin oil | ?0.1％ | 99％ | |
| 8 | Machine oil | ?0.3％ | 97％ | |
| 9 | No. 200 solvents | ?0.2％ | 98％ |
Know from above-mentioned experimental result:
(1) liquid-gas ratio is to the influence of absorptivity.Know the rising with liquid-gas ratio from table 1, absorptivity also increases.Fix (to a specific absorption tower) when mass-transfer efficiency, liquid-gas ratio is low more, CS
2Content in paraffin oil is high, and its saturated vapor pressure is high more, H after absorption is accomplished
2CS in the S gas
2Content is high more.
(2) mixed raw material gas pressure is to the influence of absorptivity.There is an optimum value in mixed raw material gas pressure, and at the optimum value place, absorptivity can reach 99%, and it is low to consume energy, conserve energy.
(3) absorb back CS
2Concentration lower.The top balanced gas that absorbs back mineral oil liquid is carried out chromatography-mass spectroscopy detect, can know CS in the gas after the absorption by testing result
2Concentration drop to 0.1%～0.8% by initial 10%, can be used for the reaction of follow-up synthesis of methyl mercaptan, and influence is very little.
Claims (5)
1. device with carbon disulfide in the solvent absorbing hydrogen sulphide gas; Mainly comprise absorption tower (1), Analytic Tower (2), the 1st gas-liquid separator (3) and the 2nd gas-liquid separator (4), it is characterized in that heat exchanger (5), cooler (6), heater (7) in addition, described absorption tower (1) thin upper and lower two sections for thick down; Bottom one side of the hypomere of (1) is provided with a through hole on the absorption tower; This through hole is communicated with the inner chamber of absorption tower (1) hypomere through the 1st flow control valve, the 1st three-way pipe and the tube connector of band flowmeter with the mixed raw material gas generation device, mixed raw material gas is through the bottom of tube connector through the straight tube entering absorption tower (1) of the 1st flow control valve of band flowmeter and the 1st three-way pipe, and is mobile from bottom to top in absorption tower (1); The bottom centre of (1) place is provided with a through hole on the absorption tower; This through hole is communicated with the arm of the 2nd three-way pipe through the straight tube and the tube connector of the 2nd three-way pipe with the import of booster pump (9); Be communicated with through the import of tube connector with circulating pump (8); The outlet of circulating pump (8) is communicated with the through hole that hypomere top, absorption tower (1) one side is provided with through the 2nd flow control valve and the tube connector of band flowmeter, is positioned over the part of the solvent of absorption tower (1) hypomere through hole, under the effect of circulating pump (8); Get into the top of absorption tower (1) hypomere through this through hole; In the hypomere of absorption tower (1), after liquid distribution trough disperses, flow from the top down, fully contact, absorb the carbon disulfide in the mixed raw material gas with the mixed raw material gas that flows from bottom to top; The outlet of booster pump (9) is communicated with the interior pipe import of heat exchanger (5) through the 3rd flow control valve and tube connector; The outlet of the interior pipe of heat exchanger (5) is communicated with the through hole that Analytic Tower (2) top one side is provided with through tube connector, and the solvent that is absorbed with carbon disulfide passes through heat exchanger (5) preheating after this through hole gets into the top of Analytic Tower (2) epimere, after liquid distribution trough disperses; In Analytic Tower (2), flow from top to bottom and emit carbon disulfide and regenerate; Top one side of (1) epimere is provided with a through hole on the absorption tower, and the solvent after Analytic Tower (2) regeneration and the solvent after the 1st gas-liquid separator (3) separates get into the top on absorption tower (1), and mobile from the top down in absorption tower (1); Fully contact with the gas that flows from bottom to top; The center, top of (1) is provided with a through hole on the absorption tower, and this through hole is communicated with the through hole that the 1st gas-liquid separator (3) one sides are provided with through tube connector, and a through hole that removes hydrogen sulfide gas (1) top through the absorption tower of carbon disulfide in absorption tower (1) gets into the 1st gas-liquid separator (3); In the 1st gas-liquid separator (3), carry out gas-liquid separation; The through hole that liquid after the separation is provided with through the 1st gas-liquid separator (3) bottom centre place is by the arm of the 4th flow control valve of band liquid level gauge and tube connector and the 3rd three-way pipe mixes entering absorption tower (1), back epimere with the regenerated solvent that comes from Analytic Tower (2) top, gets back in the absorption tower (1) to absorb carbon disulfide again, the through hole and the tube connector collection of gas warp the 1st gas-liquid separator (3) the top center place setting after the separation;
Described Analytic Tower (2) is divided into upper and lower two sections; Raise through rich solution temperature behind heat exchanger (5) that booster pump (9) transports from absorption tower (1); Through hole through Analytic Tower (2) epimere one side gets into Analytic Tower (2) again; And after liquid distribution trough disperses, in Analytic Tower (2), flow from top to bottom, on Analytic Tower (2) top; The part parsing takes place in carbon disulfide in the rich solution; At last pars infrasegmentalis one side of Analytic Tower (2) and the homonymy on hypomere top, a through hole is set respectively, this two through hole is communicated with the two ends of pipe in the heater (7) through tube connector respectively; In heater (7), be provided with thermocouple thermometer on the tube connector of pipe outlet simultaneously; The rich solution that heater (7) is partly resolved for the carbon disulfide that comes from Analytic Tower (2) epimere provides heat, and the through hole of the rich solution after the heating through Analytic Tower (2) hypomere top is back in the Analytic Tower (2), after liquid distribution trough disperses; Resolve to lean solution at the mobile from top to bottom one-step removal carbon disulfide of going forward side by side of Analytic Tower (2) hypomere; The through hole on pipe, epimere top, absorption tower (1) gets into absorption tower (1) in the 5th flow control valve of the through hole that the lean solution after Analytic Tower (2) is resolved is provided with through Analytic Tower (2) bottom centre place, tube connector, band liquid level gauge, the heat exchanger (5), and the carbon disulfide after Analytic Tower (2) is resolved is at first removed entrained liquid at the demister that Analytic Tower (2) inner top is provided with; The through hole and the tube connector that are provided with through Analytic Tower (2) top center place then communicate with the interior pipe import of cooler (6); The outlet of pipe is communicated with the through hole that a side of the 2nd gas-liquid separator (4) is provided with through tube connector in the cooler (6), on the tube connector of cooler (6) outlet, thermocouple thermometer is set, in the 2nd gas-liquid separator (4); Cooled carbon disulfide liquid carries out gas-liquid separation with the carbon disulfide gas that contains a small amount of hydrogen sulfide, the through hole that the gas after the separation is provided with through the 2nd gas-liquid separator (4) top center place, tube connector, with the arm of manometric the 6th flow control valve, the 1st three-way pipe and entering absorption tower (1) hypomere after mixed raw material gas mixes; The isolated carbon disulfide liquid of the 2nd gas-liquid separator (4), the 7th flow control valve of through hole that is provided with through the 2nd gas-liquid separator (4) bottom centre place and tube connector and band liquid level gauge is collected;
Described heat exchanger (5) is conventional tubular heat exchanger; Described heater (7) is conventional shell and tube steam heater; Described cooler (6) is conventional shell and tube water cooler.
2. method with carbon disulfide in the solvent absorbing hydrogen sulphide is characterized in that concrete method step is following:
(1) absorbs
With the initial concentration of carbon disulfide is 10%, and pressure is the mixed raw material gas of 0.2～0.4MPa, the bottom one side through hole input of (1) hypomere from the absorption tower; In absorption tower (1), flow from bottom to top, be positioned over the solvent of absorption tower (1), i.e. paraffin oil or machine oil or No. 200 solvents; Be forced into 0.25～0.45MPa through circulating pump (8), the through hole of (1) the hypomere top one side input from the absorption tower is behind liquid distribution trough; In the hypomere of absorption tower (1), spray from the top down; And from the circulation lean solution of Analytic Tower (2) bottom, the through hole of top one side of (1) epimere input from the absorption tower, through behind the liquid distribution trough in absorption tower (1) spray from the top down; Fully contact with the mixed raw material gas that flows from bottom to top and absorb carbon disulfide, solvent: the mass ratio of mixed raw material gas is 1: 0.72～2.8;
(2) resolve
After the completion of (1) step, (1) step of warp in absorption tower (1) is absorbed with the part of the solvent of carbon disulfide, is pressurized to 0.3～0.5MPa through booster pump (9) earlier; After heat exchanger (5) carries out preheating; Be preheated to 110～130 ℃, get into the epimere of Analytic Tower (2) then through tube connector, in tower, flow from top to bottom through liquid distribution trough; After resolving; Be heated to 120～140 ℃ through heater (7) again, further fully resolve and become lean solution at the hypomere of Analytic Tower (2), last lean solution is delivered to heat exchanger (5) from the bottom through-hole output of Analytic Tower (2) and through tube connector; Be cooled to 30～35 ℃ through heat exchanger (5) heat exchange, get in the absorption tower (1) through the through hole of tube connector again through epimere top, absorption tower (1) one side;
(3) gas-liquid separation
After the completion of (1) step; In absorption tower (1); (1) step of warp solvent has absorbed the hydrogen sulfide gas of carbon disulfide, and the through hole and the tube connector at (1) top through the absorption tower are imported the 1st gas-liquid separator (3) and carried out gas-liquid separation; Gas after the separation is finished product, collects through the through hole and the tube connector output at the 1st gas-liquid separator (3) top; Liquid after the separation through the through hole of the 1st gas-liquid separator (3) bottom and the through hole of tube connector and epimere top, absorption tower (1) one side, gets in the absorption tower (1);
In Analytic Tower (2); Gas after (2) step resolved is delivered to manage in the cooler (6) with tube connector through the through hole at Analytic Tower (2) top and is cooled to 5～10 ℃; Get into the 2nd gas-liquid separator (4) from the 2nd gas-liquid separator (4) one side through hole and carry out gas-liquid separation, the liquid after the separation is collected through the bottom through-hole and the tube connector output of the 2nd gas-liquid separator (4); To the gas after separating through the arm of through hole, tube connector, band Pressure gauge the 6th flow control valve and the 1st three-way pipe at the 2nd gas-liquid separator (4) top with after mixed raw material gas mixes; Through the through hole of pars infrasegmentalis one side under absorption tower (1), get into absorption tower (1) recirculation.
3. according to the described method of claim 2, it is characterized in that with carbon disulfide in the solvent absorbing hydrogen sulphide:
In (1) step, the pressure of mixed raw material gas is 0.3MPa, and the solvent of absorption tower (1) is a paraffin oil, and circulating pump is forced into 0.35 MPa, the paraffin oil solvent: the mass ratio of mixed raw material gas is 1: 2.8;
In (2) step, booster pump is pressurized to 0.4MPa, and solvent is that 120 ℃ and heater via are heated to 130 ℃ through the temperature of heat exchanger (5) preheating, and lean solution is cooled to 30 ℃ through heat exchanger;
In (3) step, the gas after the parsing is cooled to 6 ℃ through cooler.
4. according to the described method of claim 2, it is characterized in that with carbon disulfide in the solvent absorbing hydrogen sulphide:
In (1) step, the pressure of mixed raw material gas is 0.3MPa, and the solvent of absorption tower (1) is a machine oil, and circulating pump is forced into 0.35MPa, the machine oil solvent: the mass ratio of mixed raw material gas is 1: 2.8;
In (2) step, booster pump is pressurized to 0.4MPa, and solvent is that 120 ℃ and heater via are heated to 130 ℃ through the temperature of heat exchanger (5) preheating, and lean solution is cooled to 35 ℃ through heat exchanger;
In (3) step, the gas after the parsing is cooled to 10 ℃ through cooler.
5. according to the described method of claim 2, it is characterized in that with carbon disulfide in the solvent absorbing hydrogen sulphide:
In (1) step, the pressure of mixed raw material gas is 0.3MPa, and the solvent of absorption tower (1) is No. 200 solvents, and circulating pump is forced into 0.35MPa, No. 200 solvents: the mass ratio of mixed raw material gas is 1: 2.8;
In (2) step, booster pump is pressurized to 0.4MPa, and solvent is that 120 ℃ and heater via are heated to 130 ℃ through the temperature of heat exchanger (5) preheating, and lean solution is cooled to 35 ℃ through heat exchanger;
In (3) step, the gas after the parsing is cooled to 10 ℃ through cooler.
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| FR2900842B1 (en) * | 2006-05-10 | 2009-01-23 | Inst Francais Du Petrole | PROCESS FOR DEACIDIFYING A GASEOUS EFFLUENT WITH EXTRACTION OF PRODUCTS TO BE REGENERATED |
| CN201308807Y (en) * | 2008-12-01 | 2009-09-16 | 李怀毅 | Retracting device of carbon disulfide in carbon disulfide tail gas in semi-coking method production |
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| US9993766B2 (en) | 2014-11-14 | 2018-06-12 | Kabushiki Kaisha Toshiba | Carbon dioxide capture apparatus and method of capturing carbon dioxide |
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