CN104524938A - Device and method for alkali-free desulfuration and deodorization by virtue of liquefied gas fixed bed - Google Patents
Device and method for alkali-free desulfuration and deodorization by virtue of liquefied gas fixed bed Download PDFInfo
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Abstract
The invention relates to a device for alkali-free desulfuration and deodorization by virtue of a liquefied gas fixed bed. The device comprises a first desulfuration agent tank, a first path of porcelain balls, a second path of porcelain balls, a catalyst tank, a third path of porcelain balls, a fourth path of porcelain balls, a second desulfuration agent tank, a fifth path of porcelain balls and a sixth path of porcelain balls, wherein a liquefied gas inlet is formed in the bottom of the first desulfuration agent tank, a first desulfuration agent region is formed between the first path of porcelain balls and the second path of porcelain balls, a catalyst region is formed between the third path of porcelain balls and the fourth path of porcelain balls, a second desulfuration agent region is formed between the fifth path of porcelain balls and the sixth path of porcelain balls, and a liquefied gas outlet is formed in the top of the second desulfuration agent tank; the first desulfuration agent region and the second desulfuration agent region are filled with the same desulfurizing agents, and the catalyst region is filled with an organic sulfur conversion catalyst. The invention further relates to a method for alkali-free desulfuration and deodorization by virtue of a liquefied gas fixed bed by the device. According to the device and the method, alkali liquid does not need to be prepared, alkali slag does not need to be discharged, the environmental pollution caused by the discharging of the alkali slag is avoided, a liquefied gas product is stable in quality, the operation is convenient, the process is simple, and power and other aids are not needed.
Description
Technical field
The present invention relates to liquefied gas technical field of refinement in petroleum refining process, particularly a kind of device and method of liquefied gas fixed bed alkali-free desulfuration-deodorization.
Background technology
Liquefied petroleum gas is one of product in petroleum refining process, is also the important source material being processed into other products further.Refined material liquefied petroleum gas is mainly with the liquefied gas after alcohol amine removal of H2S, the liquefied gas main component come from hydramine method desulfurization unit is C3, C4 component, containing a small amount of hydrogen sulfide and organic sulfur (mainly mercaptan, cos, carbon disulfide).
Liquefied gas reforming catalyst in the market mainly contain sulfonated phthalocyanine cobalt and or poly-phthalocyanine cobalt catalyst, but these two kinds of catalyst only have good transformation to sodium mercaptides, function singleness, and need another fresh air and or activator, complex process, cost is high.
Existing liquefied gas purification techniques, general adopts Merox extracting-liquid phase catalytic oxidation technique, in extraction tower, the mercaptan in liquefied gas and agent aqueous slkali (sulfonated phthalocyanine cobalt alkali lye) react generate sodium mercaptides and transfer to alkali mutually in; Agent alkali lye after being separated with liquefied gas enters oxidation regeneration tower, and under air effect, the sodium mercaptides in alkali lye is oxidized to disulphide, realizes removing of mercaptan, and alkali lye, catalyst regeneration, recycle simultaneously.But there are the following problems for this technique: 1) can produce a large amount of alkaline residues, alkaline residue has serious foul odour, can cause environmental problem; 2) because alkaline residue does not thoroughly produce with being separated of liquefied gas, product liquefied gas is defective (harmful substance exceeds standard and causes) often; 3) process alkaline residue and will spend a large amount of human and material resources, and there is secondary pollution, sulphur is discharged in air in the form of the oxide and can causes air pollution; 4) operation exists hidden danger, when joining alkali lye, caustic soda and alkali lye are easily hurted sb.'s feelings, and when unloading alkaline residue, easily cause gas leak.
Summary of the invention
The object of the invention is to overcome above-mentioned the deficiencies in the prior art, there is provided a kind of technique simple, easy to operate, discharge without alkaline residue, effectively can remove a small amount of hydrogen sulfide in liquefied gas, and effectively transform, the method for the fixed bed desulfuration-deodorization of the organic sulfur (mainly mercaptan, cos, carbon disulfide) removed in liquefied gas and device.
The technical scheme that the present invention realizes its object is as follows:
A kind of device of liquefied gas fixed bed alkali-free desulfuration-deodorization, comprise the first desulfurizing agent tank, first porcelain ball, second porcelain ball, catalyst tank, 3rd road porcelain ball, 4th road porcelain ball, second desulfurizing agent tank, 5th road porcelain ball, 6th road porcelain ball, the bottom of the first desulfurizing agent tank is provided with liquefied gas entrance, first porcelain ball is positioned at the bottom of the first desulfurizing agent tank, second porcelain ball is positioned at the top of the first desulfurizing agent tank, it is the first desulfurizing agent district between first porcelain ball and second porcelain ball, the top exit of the first desulfurizing agent tank is connected by pipeline with the bottom inlet of catalyst tank, 3rd road porcelain ball is positioned at the bottom of catalyst tank, and the 4th road porcelain ball is positioned at the top of catalyst tank, is catalyst zone between the 3rd road porcelain ball and the 4th road porcelain ball, and the top exit of catalyst tank is connected by pipeline with the bottom inlet of the second desulfurizing agent tank, 5th road porcelain ball is positioned at the bottom of the second desulfurizing agent tank, and the 6th road porcelain ball is positioned at the top of the second desulfurizing agent tank, is the second desulfurizing agent district between the 5th road porcelain ball and the 6th road porcelain ball, and the top of the second desulfurizing agent tank is provided with liquefied gas outlet,
Described first desulfurizing agent district is identical with the desulfurizing agent that the second desulfurizing agent district fills, and described desulfurizing agent is made up of the following component of percentage by weight: ZnO:35 ~ 50%, MnO
2: 35 ~ 50%, CaO:5 ~ 15%, surplus is carrier, and described carrier is made up of the aluminum oxide of 40 ~ 65% and the silica of 35 ~ 60%;
The organic sulfur conversion catalyst that described catalyst zone is filled is made up of the following component of percentage by weight: Ni:10 ~ 20%, Na
2o:5 ~ 10%, surplus is γ-Al
2o
3carrier.
The active porcelain ball that described first porcelain ball, second porcelain ball, the 3rd road porcelain ball, the 4th road porcelain ball, the 5th road porcelain ball and the 6th road porcelain ball are diameter 6 ~ 10mm stacks together.
Described first porcelain ball, second porcelain ball, the 3rd road porcelain ball, the 4th road porcelain ball, the 5th road porcelain ball and the 6th road porcelain ball by etc. the diameter of mass ratio be 6 and the active porcelain ball of 10mm stack together.
Described ZnO derive from activated zinc oxide, basic zinc carbonate, zinc carbonate one or more; Described MnO
2derive from manganese carbonate, activity oxidation manganese, manganese acetate one or more; Described CaO derive from calcium hydroxide, calcium carbonate, calcium acetate one or more; One or more in aluminium hydroxide, thin water aluminium, aluminium oxide of described aluminum oxide source.
Described Ni derive from nickel nitrate, nickelous sulfate, nickel chloride, nickel acetate one or more; Na
2o derive from NaOH, sodium carbonate, sodium acetate one or more.
During use, multiple fixed bed bed can be designed as required, hydrogen sulfide content in pending liquefied gas is not more than 5PPm, liquid gas flow through one or more organic sulfur conversion beds, then flows through one or more sulfur absorbing agent bed.
Utilize said apparatus to be fixed a method for alkali-free desulfuration-deodorization to liquefied gas, comprise the steps:
1) liquefied gas come from hydramine method desulfurization unit is inputted from the liquefied gas entrance of the first desulfurizing agent pot bottom, liquefied gas is first through first porcelain ball, desulfurizing agent again through the first desulfurizing agent district removes the hydrogen sulfide in liquefied gas, then through second porcelain ball, export from the first desulfurizing agent tank top;
2) liquefied gas exported from the first desulfurizing agent tank top enters catalyst tank by pipeline from the bottom inlet of catalyst tank, through the 3rd road porcelain ball, organic sulfur conversion in liquefied gas is hydrogen sulfide and disulphide by the organic sulfur conversion catalyst then through catalyst zone, then through the 4th road porcelain ball, export from the top of catalyst tank;
3) liquefied gas exported from the top of catalyst tank enters the second desulfurizing agent tank through piping from the bottom inlet of the second desulfurizing agent tank, through the 5th road porcelain ball, then hydrogen sulfide, disulphide and carbon dioxide is removed through the second desulfurizing agent district of the second desulfurizing agent tank, then through the 6th road porcelain ball, export from the liquefied gas outlet at digester top, enter gas separation unit.
The course of work of the present invention and principle are: the liquefied gas come from hydramine method desulfurization unit, under the pressure and temperature of himself, by pipeline and valve, the first desulfurizing agent tank is entered from the liquefied gas entrance of the first desulfurizing agent pot bottom, in first desulfurizing agent tank, porcelain ball and desulfurizing agent are housed, hydrogen sulfide in liquefied gas and reactive desulfurizing agent generate metal sulfide thus remove hydrogen sulfide wherein, the hydrogen sulfide content entered in catalyst tank is made to be not more than 5PPm, with the normal performance of the catalyst performance in guard catalyst tank with ensure its service life (especially when hydrogen sulfide content is higher time), desulfurizing agent of the present invention and organic sulfur conversion catalyst have good compatibility and synergy, desulfurizing agent can assist the organic sulfur in catalytic conversion liquefied gas, liquefied gas after fine de-sulfur hydrogen exports after piping and valve enter catalyst tank from the first desulfurizing agent tank top, cos in liquefied gas and carbon disulfide react respectively with water and generate hydrogen sulfide and carbon dioxide under the effect of catalyst, mercaptan (R-SH) generates disulphide (oxygen main source is the free oxygen in liquefied gas and the component in catalyst) under the effect of catalyst with oxygen reaction, reaction equation is:
The liquefied gas of organic sulfur after catalytic conversion exports from catalyst tank top, the second desulfurizing agent tank is entered from the second desulfurizing agent pot bottom through piping and valve, desulfurizing agent carries out essence remove through organic sulfur conversion catalytic conversion hydrogen sulfide out, carbon dioxide, part physical and chemisorbed are carried out to organic sulfur conversion catalytic conversion disulphide out: hydrogen sulfide reacts respectively to zinc oxide, manganese oxide, calcium oxide and generates corresponding metal sulfide, is fixed on desulfurizing agent; The oxide of mercaptan and manganese reacts and generates Organic Manganese, and disulfide moieties is adsorbed on desulfurizing agent by chemistry, physical action; Carbon dioxide and calcium oxide react and generate calcium carbonate.Liquefied gas after desulfurization out delivers to gas separation unit through piping and valve from the outlet being located at the second desulfurizing agent tank top.
The invention has the beneficial effects as follows: (1) carries out catalyzed conversion specially to the organic sulfur (mainly mercaptan, cos, carbon disulfide) in liquefied gas, and essence is carried out to hydrogen sulfide wherein remove, also can partial removal to the disulphide transformed, the refining object of desulfuration-deodorization can better be reached; (2) environmental pollution caused is discharged without alkaline residue; (3) without the need to joining alkali lye, unloading alkaline residue, hidden danger is eliminated; (4) liquefied gas constant product quality, is conducive to further processing; (5) easy to operate, technique is simple, without increasing power and other auxiliary agent.
Accompanying drawing explanation
Fig. 1 is the apparatus structure schematic diagram of liquefied gas fixed bed alkali-free desulfuration-deodorization of the present invention;
In figure: 1, the first desulfurizing agent tank; 2, first porcelain ball; 3, second porcelain ball; 4, catalyst tank; 5, the 3rd road porcelain ball; 6, the 4th road porcelain ball; 7, the second desulfurizing agent tank; 8, the 5th road porcelain ball; 9, the 6th road porcelain ball; 10, liquefied gas entrance; 11, the first desulfurizing agent district; 12, catalyst zone; 13, the second desulfurizing agent district; 14, liquefied gas outlet.
Detailed description of the invention
As shown in Figure 1, the device of liquefied gas fixed bed alkali-free desulfuration-deodorization of the present invention, by the first desulfurizing agent tank 1, first porcelain ball 2, second porcelain ball 3, catalyst tank 4, 3rd road porcelain ball 5, 4th road porcelain ball 6, second desulfurizing agent tank 7, 5th road porcelain ball 8 and the 6th road porcelain ball 9 form, the bottom of the first desulfurizing agent tank 1 is provided with liquefied gas entrance 10, first porcelain ball 2 is positioned at the bottom of the first desulfurizing agent tank 1, second porcelain ball 3 is positioned at the top of the first desulfurizing agent tank 1, it is the first desulfurizing agent district 11 between first porcelain ball 2 and second porcelain ball 3, the top exit of the first desulfurizing agent tank 1 is connected with valve by pipeline with the bottom inlet of catalyst tank 4, 3rd road porcelain ball 5 is positioned at the bottom of catalyst tank 4,4th road porcelain ball 6 is positioned at the top of catalyst tank 4, be catalyst zone 12 between 3rd road porcelain ball 5 and the 4th road porcelain ball 6, the top exit of catalyst tank 4 is connected with valve by pipeline with the bottom inlet of the second desulfurizing agent tank 7, 5th road porcelain ball 8 is positioned at the bottom of the second desulfurizing agent tank 7, and the 6th road porcelain ball 9 is positioned at the top of the second desulfurizing agent tank 7, is that the top of the second desulfurizing agent district 13, second desulfurizing agent tank 7 is provided with liquefied gas and exports 14 between the 5th road porcelain ball 8 and the 6th road porcelain ball 9.
First porcelain ball 2, second porcelain ball the 3, the 3rd road porcelain ball the 5, the 4th road porcelain ball the 6, the 5th road porcelain ball 8 and the 6th road porcelain ball 9 are diameter to be 10 millimeters and diameter be 6 millimeters active porcelain ball by etc. mass ratio with the use of.
First desulfurizing agent district 11 is identical with the desulfurizing agent that the second desulfurizing agent district 13 fills, and is made up of: ZnO:35 ~ 50%, MnO the following component of percentage by weight
2: 35 ~ 50%, CaO:5 ~ 15%, surplus is carrier, and carrier is made up of the aluminum oxide of 40 ~ 65% and the silica of 35 ~ 60%.Described ZnO derive from activated zinc oxide, basic zinc carbonate, zinc carbonate one or more; Described MnO
2derive from manganese carbonate, activity oxidation manganese, manganese acetate one or more; Described CaO derive from calcium hydroxide, calcium carbonate, calcium acetate one or more; One or more in aluminium hydroxide, thin water aluminium, aluminium oxide of described aluminum oxide source.
The organic sulfur conversion catalyst that catalyst zone 12 is filled is made up of the following component of percentage by weight: Ni:10 ~ 20%, Na
2o:5 ~ 10%, surplus is γ-Al
2o
3carrier; Described Ni derive from nickel nitrate, nickelous sulfate, nickel chloride, nickel acetate one or more; Na
2o derive from NaOH, sodium carbonate, sodium acetate one or more.
Utilize said apparatus to be fixed a method for alkali-free desulfuration-deodorization to liquefied gas, operate in accordance with the following steps:
1) liquefied gas come from hydramine method desulfurization unit is inputted from the liquefied gas entrance 10 bottom the first desulfurizing agent tank 1, liquefied gas is first through first porcelain ball 2, desulfurizing agent again through the first desulfurizing agent district 11 removes the hydrogen sulfide in liquefied gas, then through second porcelain ball 3, export from the first desulfurizing agent tank 1 top.First desulfurizing agent tank 1 plays the catalyst in guard catalyst tank 4, reduces hydrogen sulfide content, makes to enter hydrogen sulfide in the liquefied gas of catalyst not higher than 5PPm, and to make catalyst stabilization, efficient, long-life plays a role.
2) liquefied gas exported from the first desulfurizing agent tank 1 top enters catalyst tank 4 by pipeline from the bottom inlet of catalyst tank 4, through the 3rd road porcelain ball 5, organic sulfur conversion in liquefied gas is hydrogen sulfide and disulphide by the organic sulfur conversion catalyst then through catalyst zone 12, then flow through the 4th road porcelain ball 6, export from the top of catalyst tank 4.
3) liquefied gas exported from the top of catalyst tank 4 enters the second desulfurizing agent tank 7 through piping from the bottom inlet of the second desulfurizing agent tank 7, through the 5th road porcelain ball 8, then hydrogen sulfide, disulphide and carbon dioxide is removed through the second desulfurizing agent district 13 of the second desulfurizing agent tank 7, then through the 6th road porcelain ball 9, export from the liquefied gas outlet 14 at digester top, enter gas separation unit.
Application example:
Utilize said apparatus and method to carry out liquefied gas fixed bed alkali-free desulfuration-deodorization, every one porcelain ball all containing the porcelain ball of 0.5 ton 6 millimeters and the porcelain ball of 0.5 ton 10 millimeters, liquefied gas in porch first through excessive porcelain ball again through too small porcelain ball, then contrary in exit.The diameter of the first desulfurizing agent tank is 2400 millimeters, the canned desulfurizing agent 58.3m of the first desulfurizing agent
3, the loading height of desulfurizing agent is 12900 millimeters.The diameter of catalyst tank is 2400 millimeters, catalyst canning organic sulfur conversion catalyst 39.0m
3, the loading height of catalyst is 8600 millimeters.Second desulfurizing agent tank diameter is 2400 millimeters, the tanked liquefied gas desulfurizer 58.3m of the second desulfurizing agent
3, desulfurizing agent loading height is 12900 millimeters.By the liquefied gas from alcohol amine removal of H2S, (hydrogen sulfide content is 12.4mg/m
3, mercaptans content is 189mg/m
3, COS content is 14.5mg/m
3, carbon disulfide 4.86mg/m
3, total sulfur is 221mg/m
3) from the speed input by 32.25 tons/hour of the liquefied gas entrance 10 of the first desulfurizing agent tank 1, the liquefied gas hydrogen sulfide content after apparatus of the present invention and method purification is for being less than 1mg/m
3, mercaptans content is 8.36mg/m
3, COS content is less than 0.1mg/m
3, carbon disulfide content is less than 0.1mg/m
3, copper corruption is 1a, total sulfur 101mg/m
3, greatly reduce the sulfur content in liquefied gas.The service life of desulfurizing agent and catalyst is 3 years, long service life.
Use apparatus and method of the present invention, thoroughly solve the emission problem of liquefied gas alkaline mud, there is no the problem of secondary pollution, meet environmental requirement; Without joining alkali lye and unloading alkaline residue two procedures, do not wash the waste water after alkali lye yet, eliminate potential safety hazard; Technological operation is convenient, simple, without the need to supplementary air, other auxiliary agent and extra power; Alleviate labor strength, also convenient management.
Claims (6)
1. the device of a liquefied gas fixed bed alkali-free desulfuration-deodorization, it is characterized in that, comprise the first desulfurizing agent tank (1), first porcelain ball (2), second porcelain ball (3), catalyst tank (4), 3rd road porcelain ball (5), 4th road porcelain ball (6), second desulfurizing agent tank (7), 5th road porcelain ball (8), 6th road porcelain ball (9), the bottom of the first desulfurizing agent tank (1) is provided with liquefied gas entrance (10), first porcelain ball (2) is positioned at the bottom of the first desulfurizing agent tank (1), second porcelain ball (3) is positioned at the top of the first desulfurizing agent tank (1), it is the first desulfurizing agent district (11) between first porcelain ball (2) and second porcelain ball (3), the top exit of the first desulfurizing agent tank (1) is connected by pipeline with the bottom inlet of catalyst tank (4), 3rd road porcelain ball (5) is positioned at the bottom of catalyst tank (4), 4th road porcelain ball (6) is positioned at the top of catalyst tank (4), be catalyst zone (12) between 3rd road porcelain ball (5) and the 4th road porcelain ball (6), the top exit of catalyst tank (4) is connected by pipeline with the bottom inlet of the second desulfurizing agent tank (7), 5th road porcelain ball (8) is positioned at the bottom of the second desulfurizing agent tank (7), 6th road porcelain ball (9) is positioned at the top of the second desulfurizing agent tank (7), be the second desulfurizing agent district (13) between 5th road porcelain ball (8) and the 6th road porcelain ball (9), the top of the second desulfurizing agent tank (7) is provided with liquefied gas outlet (14),
Described first desulfurizing agent district (11) is identical with the desulfurizing agent that the second desulfurizing agent district (13) fills, and described desulfurizing agent is made up of the following component of percentage by weight: ZnO:35 ~ 50%, MnO
2: 35 ~ 50%, CaO:5 ~ 15%, surplus is carrier, and described carrier is made up of the aluminum oxide of 40 ~ 65% and the silica of 35 ~ 60%;
The organic sulfur conversion catalyst that described catalyst zone (12) is filled is made up of the following component of percentage by weight: Ni:10 ~ 20%, Na
2o:5 ~ 10%, surplus is γ-Al
2o
3carrier.
2. the device of liquefied gas fixed bed alkali-free desulfuration-deodorization as claimed in claim 1, it is characterized in that, it is that the active porcelain ball of 6 ~ 10mm stacks together that described first porcelain ball (2), second porcelain ball (3), the 3rd road porcelain ball (5), the 4th road porcelain ball (6), the 5th road porcelain ball (8) and the 6th road porcelain ball (9) are diameter.
3. the device of liquefied gas fixed bed alkali-free desulfuration-deodorization as claimed in claim 2, it is characterized in that, described first porcelain ball (2), second porcelain ball (3), the 3rd road porcelain ball (5), the 4th road porcelain ball (6), the 5th road porcelain ball (8) and the 6th road porcelain ball (9) by etc. the diameter of mass ratio be 6 and the active porcelain ball of 10mm stack together.
4. the device of liquefied gas fixed bed alkali-free desulfuration-deodorization as claimed in claim 1, is characterized in that, described ZnO derive from activated zinc oxide, basic zinc carbonate, zinc carbonate one or more; Described MnO
2derive from manganese carbonate, activity oxidation manganese, manganese acetate one or more; Described CaO derive from calcium hydroxide, calcium carbonate, calcium acetate one or more; One or more in aluminium hydroxide, thin water aluminium, aluminium oxide of described aluminum oxide source.
5. the device of liquefied gas fixed bed alkali-free desulfuration-deodorization as claimed in claim 1, is characterized in that, described Ni derive from nickel nitrate, nickelous sulfate, nickel chloride, nickel acetate one or more; Na
2o derive from NaOH, sodium carbonate, sodium acetate one or more.
6. carry out a method for liquefied gas fixed bed alkali-free desulfuration-deodorization with device according to claim 1, it is characterized in that comprising the steps:
1) the liquefied gas entrance (10) of the liquefied gas come from hydramine method desulfurization unit from the first desulfurizing agent tank (1) bottom is inputted, liquefied gas is first through first porcelain ball (2), desulfurizing agent again through the first desulfurizing agent district (11) removes the hydrogen sulfide in liquefied gas, then through second porcelain ball (3), export from the first desulfurizing agent tank (1) top;
2) liquefied gas exported from the first desulfurizing agent tank (1) top enters catalyst tank (4) by pipeline from the bottom inlet of catalyst tank (4), through the 3rd road porcelain ball (5), then be hydrogen sulfide and disulphide through the organic sulfur conversion catalyst of catalyst zone (12) by the organic sulfur conversion in liquefied gas, then through the 4th road porcelain ball (6), export from the top of catalyst tank (4);
3) liquefied gas exported from the top of catalyst tank (4) enters the second desulfurizing agent tank (7) through piping from the bottom inlet of the second desulfurizing agent tank (7), through the 5th road porcelain ball (8), then hydrogen sulfide, disulphide and carbon dioxide is removed through the second desulfurizing agent district (13) of the second desulfurizing agent tank (7), then through the 6th road porcelain ball (9), export (14) from the liquefied gas at digester top to export, enter gas separation unit.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115338706A (en) * | 2022-06-30 | 2022-11-15 | 山东玲珑轮胎股份有限公司 | Tire grinding device with exhaust-gas treatment system |
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Application publication date: 20150422 |