CN104946296A - Gasoline-oxidation ammonia-process desulfurization method - Google Patents
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Abstract
The invention discloses a gasoline-oxidation ammonia-process desulfurization (GOA) technique which comprises the following steps: 1) oxidation reaction: selectively oxidating sulfur-containing compounds in gasoline by using an oxidant in the presence of a catalyst to obtain an oxidation product containing sulfur dioxide reaction exhaust (gasoline with the sulfur content of not greater than 10 ppm) and a reaction exhaust containing 0.02-1% of SOx, wherein the gasoline also comprises the intermediate component of the gasoline finished product; and 2) ammonia-process desulfurization: treating the reaction exhaust by an ammonia-process desulfurization technique to convert the sulfur dioxide into an ammonium sulfate chemical fertilizer, and discharging clean gas after reaching the standard. The method has the advantages of simple process and no secondary pollution, and can be widely used in petroleum refining industry.
Description
Technical field
The present invention relates to the manufacturing technology of clean gasoline, especially relate to the method for a kind of gasoline (catalytically cracked gasoline, straight-run spirit, petroleum naphtha, coking oil) oxidize ammonia desulfurization.Belong to the technical fields such as oil refining, chemical industry, environmental protection.
Background technology
Gasoline oxidation ammonia-process desulfurization technique more and more comes into one's own.Along with the increasingly stringent of environmental regulation, require more and more stricter to vehicular engine quality of fuel in world wide, occurred " clean fuel " of low-sulfur, low aromatic hydrocarbons and low olefin-content thereupon, wherein sulphur content problem has become domestic and international Ge great refining of petroleum enterprise production low-sulfur, the particularly key problem in technology of super low sulfur vehicular engine fuel, proposes stricter requirement to vehicle fuel oil.
At present, in petroleum product production refining technology, known gasoline desulfating method, mainly sour caustic wash desulfuration, hydrogenating reduction desulfurization and adsorption desulfurize.Acid caustic wash desulfuration technical matters is simple, facility investment is relatively low, but sweetening effectiveness is poor, and oil quality is difficult to ensure, in sweetening process, the discharge of various steam is easy to cause secondary environmental pollution, and sour caustic desulfurization technlogy is seldom applied in current oil production technique; Hydrogenating reduction sweetening effectiveness is good compared with the former, but the investment of desulfurization relevant device is very large, and its reaction conditions requires also very harsh, and operation energy consumption is too large, and desulphurization cost is high, and hydrogenation reduction process/technology is as Prime-G
+technique, CDHydro/CDHDS technology, SCAN-Fining II technology, ISAL technique, thiophenic sulfur olefin alkylation (OATS) gasoline desulfur technology etc.; Adsorption desulfurize is effective, but the investment of desulfurization relevant device is very large, and loss of octane number is large, and after desulfurization, gasoline product quality reduces, as S-Zorb technology.
Gasoline desulfur of the present invention comprises catalytically cracked gasoline, straight-run spirit, petroleum naphtha, the oxidation of coking wet goods, ammonia desulfurization.
In addition, gasoline and gasoline absorbing desulfurization technology are exactly the new technology of the production low-sulfur vehicular engine fuel developed in recent years, have report to remove sulfide in petrol by molecular sieve, modified activated carbon, but cost and efficiency still have great room for improvement.
Summary of the invention
The object of the invention is, for solving shortcoming or the deficiency of the existence of existing gasoline desulfur technology: the desulfurization of being suitable for the oil product composition carrying out finished product on a large scale, high gasoline desulfur rate is realized by lower investment, running cost, and guarantee that the desulfurization degree of the catalytically cracked gasoline of sulphur content 300 ~ 3000ppm is not less than 99.8%, make gasoline product can meet state V normal benzene requirement, the SOx generated delivers to ammonia desulfuration equipment process with reaction gas, SO
2removal efficiency>=99.9%, byproduct is ammonium sulfate, clean gas qualified discharge, invest simultaneously low, technical process is simple, running cost is low, is particularly useful for large batch of suitability for industrialized production.
Technical scheme of the present invention is, a kind of gasoline oxidation ammonia-process desulfurization technique (GOA), specifically comprises two steps:
1) oxidizing reaction, in the presence of a catalyst, with oxygenant by the sulfocompound selective oxidation in gasoline, obtains oxidation products is not more than 10ppm gasoline containing sulfurous gas reaction end gas and sulphur content (amounting to into elementary sulfur); Described gasoline also comprises the inter-level of gasoline finished product; And the reaction end gas obtained containing SOx 0.02-1%;
2) ammonia process of desulfurization, described reaction end gas adopts ammonia desulfurizing process process, Sulphur Dioxide is become ammonium sulfate fertilizer, clean gas qualified discharge;
Concrete steps: after crude product gasoline, oxygenant and catalyst mix, join in oxidation reactor, the element sulphur selective oxidation that oxygenant will contain in mercaptan, thioether, thiophene-based organic sulfide under the effect of catalyzer, change into sulfurous gas, obtain sulphur content after gas-liquid separation and be not more than the gasoline product of 10ppm and the reaction end gas containing sulfurous gas;
Oxygenant and sour gasoline counter current contact, oxidation reaction process can select fixed bed, fluidized-bed, moving-bed, suspension bed form; Reaction times 15-120 minute, preferred 20-60 minute; Catalyzed reaction temperature 25 DEG C-68 DEG C, pressure 0.05-0.89MPa.
Oxidizing reaction is carried out in suspended-bed reactor; Catalyzed reaction temperature 30 DEG C-55 DEG C, 20-60 minute.
The described reaction end gas containing sulfurous gas is passed into ammonia absorption device, uses absorption liquid sulfur dioxide absorption, absorption liquid obtains solid ammonium sulfate product through concentrated, crystallization, solid-liquid separation, drying.
Under catalyzer exists, the element sulphur selective oxidation in mercaptan, thioether, thiophene-based sulfides becomes containing SOx reaction end gas by oxygenant;
Described catalyzer is acidic cpd or its mixtures such as organic acid, mineral acid, heteropolyacid, molecular sieve, also comprises molecular sieve or gac or its compound.
Described catalyzer is comprise the solid acid catalyst of phospho-molybdic acid, phospho-wolframic acid, stearic acid, acetic acid etc. or liquid acid catalyst or its compound; Described oxygenant is that air, oxygen-rich air, pure oxygen, ozone etc. are containing oxygen element gas.
Described oxygenant molar weight is 3-200 times of sulfide molar weight, content of sulfur dioxide 0.02-1% in the oxidized tail gas obtained.
Oxidizing reaction 30-55 DEG C, be filled with the suspended-bed reactor of solid acid catalyst, acid molecular sieve catalyst, feed gasoline (sulphur content 500-2000ppm) passed into from reactor head with uniform flux, air (or oxygen-rich air) passes into from reactor lower part or side lower with uniform rate; Reaction times is 35-60min, and the gasoline after desulfurization is from bottom discharge, and sulphur content is below 10ppm.
The means such as intensified by ultrasonic wave or UV-light are adopted to strengthen to oxidation reaction process in reactor.
The tail gas containing sulfurous gas after oxidation is discharged from reactor head, sends ammonia thionizer ammonia absorption device to.
During the ammonia process of desulfurization, sweetening agent is the tail gas that ammonia absorption liquid absorbs containing sulfurous gas.After the ammoniumsulphate soln obtained is accumulated to finite concentration after evaporative crystallization, solid-liquid separation, obtain ammonium sulfate solids after drying, reach the requirement of GB acceptable end product, nitrogen content 21.1%; Sweetening agent is 0.5%-35% ammoniacal liquor or liquefied ammonia.
Absorption tower is different according to the reaction end gas sulphur oxide SOx amount of removing, concentration, and the parameter such as composition, internal circulating load of adjustment absorption liquid, guarantees assimilation effect.
Beneficial effect of the present invention: the present invention is a kind of gasoline oxidation ammonia-process desulfurization technique, and desulfuration efficiency is high, gasoline product can meet state V normal benzene requirement, invest low, running cost is low, three-waste free discharge, non-secondary pollution, the complete resource achieving element sulphur reclaims.
Apparatus of the present invention turndown ratio is very large, can adapt to catalytically cracked gasoline and straight-run spirit, petroleum naphtha, the coking oil of sulphur content 300 ~ 3000ppm.
The present invention can by more difficult for the traditional method thiophene-type sulfide effective elimination removed, and reaction conditions relaxes, and simple to operate, cost is lower, can realize heavy industrialization application.The shortcomings such as avoid traditional hydrogenation reaction flow process complicated, investment is large, severe reaction conditions, and after hydrogenation Gas-treating processes route is complicated; Also overcome the long flow path of conventional oxidation requirements of process extraction agent or sorbent material separation of oxygenated state organosulfur compound, consume large and residue to shortcomings such as gasoline quality impacts.
Gasoline oxidation ammonia desulfurization technology of the present invention, realizes more than 99.8% desulfuration efficiency, the SO of generation by lower investment and running cost
2ammonia desulfuration equipment process is sent, SO with reaction end gas
2removal efficiency>=99.9%, byproduct is ammonium sulfate, clean gas qualified discharge.Technical process is simple, and easy and simple to handle, plant running is stablized, and avoids some shortcomings of traditional technology, defines exclusive advantage.Ammonia desulfuration equipment desulfuration efficiency is not less than 99.9%, non-secondary pollution.
Accompanying drawing explanation
Fig. 1 is schema of the present invention.
Embodiment
Concrete technology step of the present invention is as follows:
1, catalyzed reaction
Fixed bed catalytic reactor adopt in industry generally adopt with acidic cpds such as organic acid, mineral acid, heteropolyacid, molecular sieves for catalyzer, with air, oxygen-rich air, oxygen, ozone for oxygenant, guaranteeing catalyzed reaction transformation efficiency by controlling temperature of reaction, pressure, reaction times, type of reactor, the way of contact etc., ensureing that the sulphur atom transformation efficiency in the thiophene of the sulfur-bearing in gasoline, thionaphthene, mercaptan, thioether equimolecular is not less than 99.8%; Its selective catalysis reaction equation is similar is:
The SOx that reaction generates departs from reaction system in time with reaction end gas, promotes constantly carrying out of catalyzed reaction.
2, the ammonia process of desulfurization
With liquefied ammonia or ammoniacal liquor as absorption agent, under suitable operational condition, in absorption tower, SOx in flue gas is removed, decreasing ratio more than 99.9%.Absorption tower is different according to SOx concentration in flue gas, is divided into 3-6 section to absorb, and partially absorbs liquid and remove ammonium sulfate after-treatment system after concentrated, solid-liquid separation, drying.
This some processes and equipment quote the authorized patent of my company.As CN200510040801.1, CN200310040801.1, CN201010275966 etc.
Schematic flow sheet is shown in Fig. 1.
Embodiment 1
At 0.1MPa (G), under 30 DEG C of reaction conditionss, be filled with the suspended-bed reactor of 100g acetic acid, sulfuric acid, molecular sieve mixed catalyst, gasoline (sulphur content 1750ppm) is passed into from reactor head with 1.5L/h speed, air passes into from reactor bottom with 40L/h speed, gasoline product after desulfurization is from bottom discharge, and sulphur content is 8.2ppm after testing.
The reaction end gas containing SOx 0.46% after catalytic oxidation is discharged from reactor head, and send ammonia desulfuration equipment, absorption agent is 11% ammoniacal liquor, the proportion 1.15g/cm of absorption liquid
3, pH5.7, internal circulating load 3.1L/h, in clean gas, content of sulfur dioxide is 30mg/Nm
3.After evaporative crystallization, solid-liquid separation, drying, obtain ammonium sulfate solids after the ammoniumsulphate soln obtained is accumulated to finite concentration, reach the requirement of GB acceptable end product, nitrogen content 21.05%.
Embodiment 2
At 0.15MPa (G), under 40 DEG C of reaction conditionss, be filled with the suspended-bed reactor of 200g oxalic acid, phosphoric acid, molecular sieve mixed catalyst, gasoline (sulphur content 1250ppm) is passed into from reactor head with 20L/h speed, 28% oxygen enrichment is adopted to pass into from reactor bottom with 200L/h speed, gasoline product after desulfurization is from bottom discharge, and sulphur content is 7.6ppm after testing.
The reaction end gas containing SOx 0.88% after catalytic oxidation is discharged from reactor head, and send ammonia desulfuration equipment, absorption agent is liquefied ammonia, the proportion 1.16g/cm of adjustment absorption liquid
3, pH6.3, internal circulating load 34.1L/h, in clean gas, content of sulfur dioxide is 25mg/Nm
3.After evaporative crystallization, solid-liquid separation, drying, obtain ammonium sulfate solids after the ammoniumsulphate soln obtained is accumulated to finite concentration, reach the requirement of GB acceptable end product, nitrogen content 21.1%.
The part that the present invention does not relate to prior art that maybe can adopt all same as the prior art is realized.Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a gasoline oxidation ammonia method desulfurizing method, is characterized in that comprising the steps:
1) oxidizing reaction, in the presence of a catalyst, with oxygenant by the sulfocompound selective oxidation in gasoline, obtains oxidation products is not more than 10ppm gasoline containing sulfurous gas reaction end gas and sulphur content; Described gasoline also comprises the inter-level of gasoline finished product; And the reaction end gas obtained containing SOx 0.02-1%;
2) ammonia process of desulfurization, described reaction end gas adopts ammonia desulfurizing process process, Sulphur Dioxide is become ammonium sulfate fertilizer, clean gas qualified discharge;
Concrete steps: after crude product gasoline, oxygenant and catalyst mix, join in oxidation reactor, the element sulphur selective oxidation that oxygenant will contain in mercaptan, thioether, thiophene-based organic sulfide under the effect of catalyzer, change into sulfurous gas, obtain sulphur content after gas-liquid separation and be not more than the gasoline product of 10ppm and the reaction end gas containing sulfurous gas.
Oxygenant and sour gasoline counter current contact, oxidation reaction process can select fixed bed, fluidized-bed, moving-bed, suspension bed form; Reaction times 15-120 minute; Catalyzed reaction temperature 25 DEG C-68 DEG C, pressure 0.05-0.89MPa.
2. gasoline oxidation ammonia method desulfurizing method according to claim 1, is characterized in that carrying out oxidizing reaction in suspended-bed reactor; Catalyzed reaction temperature 30 DEG C-55 DEG C, 20-60 minute.
3. gasoline oxidation ammonia method desulfurizing method according to claim 1, is characterized in that described catalyzer is organic acid or salt, mineral acid, heteropolyacid or salt, molecular sieve or its mixture, also comprises gac or its compound.
4. gasoline oxidation ammonia method desulfurizing method according to claim 1, is characterized in that described catalyzer is comprise phospho-molybdic acid, phospho-wolframic acid, stearic acid, the solid acid catalyst of acetic acid or liquid acid catalyst or its compound; Described oxygenant is that air, oxygen-rich air, pure oxygen, ozone etc. are containing oxygen element gas.
5. gasoline oxidation ammonia method desulfurizing method according to claim 1, is characterized in that described oxygenant molar weight is 3-200 times of sulfide molar weight, content of sulfur dioxide 0.02-1% in the oxidized tail gas obtained.
6. gasoline oxidation ammonia method desulfurizing method according to claim 1, it is characterized in that oxidizing reaction 30-55 DEG C, be filled with the suspended-bed reactor of solid acid catalyst or acid molecular sieve catalyst, feed gasoline (sulphur content 500-2000ppm) passed into from reactor head with uniform flux, air or oxygen-rich air pass into from reactor lower part or side lower with uniform rate; Reaction times is 35-60min, and the gasoline after desulfurization is from bottom discharge, and sulphur content is below 10ppm.
7. gasoline oxidation ammonia method desulfurizing method according to claim 1, is characterized in that adopting the means such as intensified by ultrasonic wave or UV-light to strengthen to oxidation reaction process in oxidation reactor.
8. gasoline oxidation ammonia method desulfurizing method according to claim 1, the described reaction end gas containing sulfurous gas is it is characterized in that to pass into ammonia absorption device, use absorption liquid sulfur dioxide absorption, absorption liquid obtains solid ammonium sulfate product through concentrated, crystallization, solid-liquid separation, drying.Sweetening agent is 0.5%-35% ammoniacal liquor or liquefied ammonia.
9. gasoline oxidation ammonia method desulfurizing method according to claim 8, is characterized in that the ammoniumsulphate soln obtained after being accumulated to finite concentration after evaporative crystallization, solid-liquid separation, obtain ammonium sulfate solids after drying.
10. gasoline oxidation ammonia method desulfurizing method according to claim 8, it is characterized in that absorption tower is different according to the reaction end gas sulphur oxide SOx amount of removing, concentration, the parameter such as composition, internal circulating load of adjustment absorption liquid, guarantees assimilation effect.
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| US10112145B1 (en) | 2017-09-07 | 2018-10-30 | Jiangnan Environmental Protection Group Inc. | Method for controlling aerosol production during absorption in ammonia desulfurization |
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| US11027234B2 (en) | 2018-04-13 | 2021-06-08 | Jiangnan Environmental Protection Group Inc. | Oxidization of ammonia desulfurization solution |
| US11224838B2 (en) | 2019-12-26 | 2022-01-18 | Jiangnan Environmental Protection Group Inc. | Controlling aerosol production during absorption in ammonia-based desulfurization |
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| US10413864B2 (en) | 2017-03-15 | 2019-09-17 | Jiangnan Environmental Protection Group Inc. | Method and apparatus for removing sulfur oxides from gas |
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