CN101747931A - Fine desulfurizing agent for transforming thioalcohol in liquid hydrocarbons at normal temperature and preparation and application methods thereof - Google Patents
Fine desulfurizing agent for transforming thioalcohol in liquid hydrocarbons at normal temperature and preparation and application methods thereof Download PDFInfo
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- CN101747931A CN101747931A CN201010028959A CN201010028959A CN101747931A CN 101747931 A CN101747931 A CN 101747931A CN 201010028959 A CN201010028959 A CN 201010028959A CN 201010028959 A CN201010028959 A CN 201010028959A CN 101747931 A CN101747931 A CN 101747931A
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Abstract
The invention relates to a fine desulfurizing agent for transforming thioalcohol in liquid hydrocarbons at the normal temperature and preparation and application methods thereof. The fine desulfurizing agent is prepared from 1 to 3 of metallic compounds including load ferric chloride, cobalt acetate, nickel acetate, copper chloride, ammonium molybdate, zinc acetate, calcium nitrate, potassium nitrate, magnesium nitrate and the like by using active carbon as a carrier. The components of the fine desulfurizing agent are based on the mass of the carrier, and the total quantity of the loaded 1 to 3 metallic compounds is 10 to 30 percent of the carrier. The preparation method for the fine desulfurizing agent comprises the following steps of: firstly, soaking the carrier by using solution of the metallic compounds; secondly, spreading the mixture, drying the mixture in the shade, and drying the mixture at the temperature of between 100 and 150 DEG C for 2 to 4 hours; and activating the mixture for 3 hours in a nitrogen atmosphere at the temperature of between 200 and 500 DEG C to obtain the fine desulfurizing agent. The fine desulfurizing agent can be widely used for transforming the thioalcohol in the liquid hydrocarbons such as liquefied petroleum gas, solvent oil, naphtha and the like, and can transform the thioalcohol in the liquid hydrocarbons into disulfides under a condition that the temperature is between 30 DEG C below zero and 180 DEG C and the space velocity is between 0.01 to 15 per hour; the removal accuracy of the thioalcohol is removed from 1,000 mgS/L to below 5 mgS/L; and the fine desulfurizing agent ensures that the sulfur capacity of the fine desulfurizing agent is 2 to 15 weight percent in the liquid hydrocarbons after treatment through a doctor experiment.
Description
Technical field:
The present invention relates to the desulfurizing agent and the methods for making and using same thereof of mercaptan in a kind of normal temperature convert liquid hydrocarbons.
Background technology:
The mercaptan that often contains different quantities in the liquid hydrocarbons such as LPG (liquefied petroleum gas (LPG)), solvent oil, petroleum naphtha, the existence of mercaptan can cause the very fast inactivation of back workshop section's catalyzer, and quality product is defective, thereby causes benefit low; Active, the easily oxidation of mercaptan character when in the liquid hydrocarbon mercaptan being arranged, not only produces stench, but also causes the decline of oil product storage stability and quality; Mercaptan has slightly acidic, and the mercaptan in the oil product is corrosive to production, bunkerage and transport pipe, and also there is the potential safety hazard in production, storage and remote the conveying simultaneously in the loss that this has not only caused corrosion to bring; Mercaptan has huge harm to human and environment, after the people sucks and to contain the air of a small amount of mercaptan, can feel headache immediately, feels sick, vomiting, symptom such as uncomfortable, and severe patient also can cause death.Mercaptan in the liquid hydrocarbon is discharged into the serious contaminate environment of meeting in the air as not adding to handle.
American UOP company had released Merox catalyzed oxidation deodorizing technology in 1958, occupied dominant position in decades at home and abroad always.This deodour method is in the presence of highly basic and catalyzer, is disulphide with air with mercaptan oxidation, and reaction is generally carried out under the temperature of normal pressure and 20～50 ℃.Catalyzer commonly used is sulfonated phthalocyanine cobalt and poly-phthalocyanine cobalt, and concentration of lye is generally 10% (w) NaOH.This deodorizing technology comprises extracting and deodorization two portions.Mercaptan is oxidized to smell and stays in the oil product with the less disulphide of harm.
Merox technology and catalyzer are worldwide used and have been done very big improvement in decades, as changing caustic alkali into weak base, use more efficiently catalyzer and activator, yet Merox technology still is not enough to satisfy fully production requirement.
It is later that the liquid hydrocarbon mercaptan of China transforms desulfurizing agent research, and domestic most of petroleum chemical enterprise adopts Merox technology, and University of Petroleum has developed AA-1 agent trace alkali deodorizing technology and catalyzer in recent years, and its deodorization principle and Merox technology are similar.
Conclusion is got up, and existing both at home and abroad deodour method and catalyzer have several aspects deficiency: deodour method that (1) is existing and catalyzer need use a large amount of alkali lye, cause having produced a large amount of salkali waste, and salkali waste processing costs height has also polluted environment; (2) in the existing deodour method, the caustic prescrub of front and the catalyzed oxidation of back are the operation of band alkali, have inevitably carried alkali lye in the oil product after the processing secretly, have influenced the quality of oil product, and have increased the weight of the corrosion to oil storage equipment; (3) existing deodour method needs the oxygenation operation, also will realize oil product and separating of alkali lye and recycling of alkali lye, causes facility investment big, complex process, process cost height; (4) utilization of Merox deodorization catalyst is the slightly acidic of mercaptan, along with the increase of thiol molecule amount, acidity more and more a little less than, high-molecular weight mercaptan can not react with alkali, thereby can not use the Merox deodorizing technology to transform.
Summary of the invention:
The objective of the invention is deficiency at existing sulfur method and catalyzer, the desulfurizing agent and the methods for making and using same thereof of mercaptan in a kind of normal temperature convert liquid hydrocarbons are provided, this desulfurizing agent can be converted into disulphide at normal temperatures with the mercaptan in the liquid hydrocarbon, remove precision for mercaptan is removed to below the 5mgS/L from 1000mgS/L, this desulfurizing agent can with the supporting use of the desulfurizing agent that removes hydrogen sulfide, can use separately again.
The objective of the invention is to realize by following method:
The desulfurizing agent of mercaptan in a kind of normal temperature convert liquid hydrocarbons, it is characterized in that, this desulfurizing agent is carrier with the gac, make for 1～3 kind in the metallic compounds such as load iron(ic) chloride, Cobaltous diacetate, nickel acetate, cupric chloride, ammonium molybdate, zinc acetate, nitrocalcite, saltpetre, magnesium nitrate, the composition of desulfurizing agent is counted with the carrier quality: described 1～3 kind of metallic compound total amount of load is 10%～30% of a carrier.
Described carrier active carbon can replace with activated alumina or molecular sieve or silica-alumina supports.
The preparation method of the desulfurizing agent of mercaptan in a kind of normal temperature convert liquid hydrocarbons of the present invention, undertaken by following steps in sequence:
1) with the metallic compound wiring solution-forming;
2) solution that 1～3 kind of metallic compound is made into is poured in the container that carrier is housed, impregnated carrier;
3) carrier that will flood metallic compound is spread out and is dried in the shade 2～4 hours;
4) carrier that will dry in the shade descended dry 2～4 hours at 100～150 ℃, and activation promptly makes this desulfurizing agent more than 3 hours under 200-500 ℃ of nitrogen atmosphere then.
This desulfurizing agent can be widely used in the conversion of mercaptan in the liquid hydrocarbons such as LPG, solvent oil, petroleum naphtha, can be with the mercaptan in the liquid hydrocarbon at-30～180 ℃ of temperature and 0.01～15h
-1Be converted into disulphide under the air speed condition, remove precision for mercaptan is removed to below the 5mgS/L from 1000mgS/L, the liquid hydrocarbon after guaranteeing to handle is tested desulfurizing agent Sulfur capacity 2-15% (wt) by doctor.
Optimizing application conditions is: at 0～150 ℃ of temperature and 0.01～15h
-1Under the air speed condition, processing contains LPG, solvent oil or the petroleum naphtha liquid hydrocarbon of mercaptan, and mercaptan is converted into disulphide, removes precision for mercaptan is removed to below the 5mgS/L from 1000mgS/L, liquid hydrocarbon after guaranteeing to handle is tested the Sulfur capacity 2%-15% (wt) of desulfurizing agent by doctor.
The brief introduction of doctor's experimental technique
Plumbic acetate or plumbous oxide are dissolved in the NaOH aqueous solution, promptly get plumbite solution.When the oil product that contains mercaptan with after plumbite solution mixes, add a certain amount of sulphur, shake 15 seconds after, static 1 minute, if the interface is pale brown or brown, promptly showing had mercaptan to exist in the oil product, doctor tests defective, represents with "+"; Otherwise doctor tests qualified, represents with "-".It is as follows that doctor tests reaction:
Pb(OH)2+2RSH＝＝(RS)2Pb+2H2O
(RS) 2Pb+S==RSSR+PbS (precipitation)
The present invention has following advantage compared with the prior art:
1) this desulfurizing agent can be widely used in the liquid hydrocarbons such as LPG, solvent oil, petroleum naphtha, and use range is wider.
2) use temperature and air speed broad, turndown ratio is big.
3) realized the alkali-free operation fully, oxygen free operation can guarantee below the outlet mercaptans content 3mgS/L, by doctor's experiment, the influence that can solve high molecular mercaptan liquid towards hydrocarbon quality fully.
4) can select variety carrier for use, as gac, activated alumina, molecular sieve or silica-alumina supports.
Embodiment
Further specify the present invention with example below:
Embodiment 1
Taking by weighing zinc acetate 14 grams is dissolved in the 60 gram water, pour into then in the beaker that 100 gram absorbent charcoal carriers are housed, solution absorption is complete, taking-up is spread out and is dried 2 hours, under 120 ℃ of conditions, dried 2.5 hours then, promptly make object-desulfurizing agent in activation under 480 ℃ of nitrogen atmospheres after 4 hours at last.
With this desulfurizing agent at 30 ℃ and 5h
-1Handle the solvent oil that contains 1000mgS/L mercaptan under the air speed, outlet mercaptans content 3mgS/L is by doctor's experiment, the Sulfur capacity 3.3% (wt) of this desulfurizing agent.
Embodiment 2
Taking by weighing nickel acetate 20 grams is dissolved in the 60 gram water, pour into then in the beaker that 100 gram absorbent charcoal carriers are housed, solution absorption is complete, taking-up is spread out and is dried 4 hours, under 140 ℃ of conditions, dried 3 hours then, promptly make object-desulfurizing agent in activation under 450 ℃ of nitrogen atmospheres after 3 hours at last.
With this desulfurizing agent at 80 ℃ and 10h
-1Handle the solvent oil that contains 1000mgS/L mercaptan under the air speed, outlet mercaptans content 4mgS/L is by doctor's experiment, the Sulfur capacity 5.3% (wt) of this desulfurizing agent.
Embodiment 3
Taking by weighing ammonium molybdate 28 grams is dissolved in the 60 gram ammoniacal liquor, pour into then in the beaker that 100 gram absorbent charcoal carriers are housed, solution absorption is complete, taking-up is spread out and is dried 2 hours, under 130 ℃ of conditions, dried 2.5 hours then, promptly make object-desulfurizing agent in activation under 320 ℃ of nitrogen atmospheres after 5 hours at last.
With this desulfurizing agent at 120 ℃ and 8h
-1Handle the petroleum naphtha that contains 1000mgS/L mercaptan under the air speed, outlet mercaptans content 3mgS/L is by doctor's experiment, the Sulfur capacity 4.3% (wt) of this desulfurizing agent.
Embodiment 4
Taking by weighing nickel acetate 5 grams and nitrocalcite 14 is dissolved in the 60 gram water, pour into then in the beaker that 100 gram absorbent charcoal carriers are housed, solution absorption is complete, taking-up is spread out and is dried 2 hours, under 150 ℃ of conditions, dried 4 hours then, promptly make object-desulfurizing agent in activation under 350 ℃ of nitrogen atmospheres after 4 hours at last.
With this desulfurizing agent at 10 ℃ and 2h
-1Handle the LPG that contains 1000mgS/L mercaptan under the air speed, outlet mercaptans content 2mgS/L is by doctor's experiment, the Sulfur capacity 7.3% (wt) of this desulfurizing agent.
Embodiment 5
Taking by weighing iron(ic) chloride 6 grams and cupric chloride 22 is dissolved in the 60 gram water, pour into then in the beaker that 100 gram absorbent charcoal carriers are housed, solution absorption is complete, taking-up is spread out and is dried 2 hours, under 100 ℃ of conditions, dried 2 hours then, promptly make object-desulfurizing agent in activation under 210 ℃ of nitrogen atmospheres after 3 hours at last.
With this desulfurizing agent at 30 ℃ and 3h
-1Handle the solvent oil that contains 1000mgS/L mercaptan under the air speed, outlet mercaptans content 3mgS/L is by doctor's experiment, the Sulfur capacity 8.5% (wt) of this desulfurizing agent.
Be applied to yueyang, hunan factory with this desulfurizing agent of producing of filling a prescription, this factory produces No. 120 solvent oils, use preceding No. 120 solvent oils of desulfurizing agent of the present invention to give out dense stink, pipeline and equipment had very strong corrodibility, product is seriously defective on indexs such as smell, colourity, can't expand market access.Applying working condition is as follows: 30000 tons/year of treatment capacities, working pressure 1.6MPa, 0～80 ℃ of temperature, import total sulfur 70～110 * 10
-6, wherein hydrogen sulfide content 3～7 * 10
-6, mercaptans content 10～20 * 10
-6Other also contains inertia sulfide, the DS-1 composite oxides desulfurizing agent that at first adopts my company to produce removes hydrogen sulfide for 4 cubic metres, then uses the 10 cubic metres of mercaptan that transform in the raw material of desulfurizing agent that relate among the present invention, and the outlet hydrogen sulfide content is stable less than 0.1 * 10
-6, mercaptans content is stable less than 1 * 10
-6, the copper corrosion of product solvent oil is less than the 1A level, and by doctor's experiment, foul smell removes fully, also not obviously influence on colourity, density.
Embodiment 6
Taking by weighing Cobaltous diacetate 4 grams and nitrocalcite 15 grams is dissolved in the 60 gram water, pour into then in the beaker that 100 gram absorbent charcoal carriers are housed, solution absorption is complete, taking-up is spread out and is dried 2 hours, under 120 ℃ of conditions, dried 2.5 hours then, promptly make object-desulfurizing agent in activation under 460 ℃ of nitrogen atmospheres after 4 hours at last.
With this desulfurizing agent at 30 ℃ and 11h
-1Handle the petroleum naphtha that contains 1000mgS/L mercaptan under the air speed, outlet mercaptans content 4mgS/L is by doctor's experiment, the Sulfur capacity 4.1% (wt) of this desulfurizing agent.
Embodiment 7
Taking by weighing Cobaltous diacetate 2 grams, magnesium nitrate 7 grams and cupric chloride 21 grams is dissolved in the 60 gram water, pour into then in the beaker that 100 gram absorbent charcoal carriers are housed, solution absorption is complete, taking-up is spread out and is dried 2 hours, under 120 ℃ of conditions, dried 2.5 hours then, promptly make object-desulfurizing agent in activation under 240 ℃ of nitrogen atmospheres after 3 hours at last.
With this desulfurizing agent at 80 ℃ and 5h
-1Handle the solvent oil that contains 1000mgS/L mercaptan under the air speed, outlet mercaptans content 3mgS/L is by doctor's experiment, the Sulfur capacity 11.3% (wt) of this desulfurizing agent.
Be applied to Nanjing factory with this desulfurizing agent of producing of filling a prescription, this factory produces Trimethylmethane, and applying working condition is as follows: 0.8～2 ton/hour of treatment capacity, working pressure 0.3～1.2MPa, temperature-10～80 ℃, import total sulfur≤20 * 10
-6, wherein hydrogen sulfide content 1～3 * 10
-6, mercaptans content 4～10 * 10
-6, the DS-1 composite oxides desulfurizing agent that at first adopts my company to produce removes hydrogen sulfide for 4 cubic metres, then uses the 5 cubic metres of mercaptan that transform in the raw material of desulfurizing agent that relate among the present invention, and the outlet hydrogen sulfide content is stable less than 0.1 * 10
-6, mercaptans content is stable less than 1 * 10
-6, the product copper corrosion after making with extra care is tested by doctor less than the 1A level.
Embodiment 8
Taking by weighing zinc acetate 7 grams, nitrocalcite 8 grams and Cobaltous diacetate 5 grams is dissolved in the 60 gram water, pour into then in the beaker that 100 gram absorbent charcoal carriers are housed, solution absorption is complete, taking-up is spread out and is dried 4 hours, under 140 ℃ of conditions, dried 4 hours then, promptly make object-desulfurizing agent in activation under 380 ℃ of nitrogen atmospheres after 3 hours at last.
With this desulfurizing agent at 130 ℃ and 11h
-1Handle the solvent oil that contains 1000mgS/L mercaptan under the air speed, outlet mercaptans content 4mgS/L is by doctor's experiment, the Sulfur capacity 12.3% (wt) of this desulfurizing agent.
Be applied to Daqing, Heilungkiang factory with this desulfurizing agent of producing of filling a prescription, annual 200000 tons of liquid light hydrocarbons, the liquid light hydrocarbon composition: C handled of this factory
10.01%, C
20.22%, C
35.98%, C
421.93%, C
524.7%, C
620.71%, C
713.78%, C
87.36%, C
93.70%, C
10 +1.61%, sulphur content in the liquid light hydrocarbon: total sulfur 140～160 * 10
-6, hydrogen sulfide 8～12 * 10
-6, mercaptan 40～70 * 10
-6, thiophene 60～80 * 10
-6, thioether 3～8 * 10
-6, carbonylsulfide 0.1～0.9 * 10
-6The product copper corrosion is greater than 3 grades before the desulfurizing agent that use the present invention relates to, and doctor's experiment is not passed through, and the product total sulfur can not satisfy relevant national standard.Operational condition is as follows: treatment capacity 45M
3/ h, working pressure 1.8-3.5MPa, temperature-5～80 ℃.The 42 cubic metres of hydrogen sulfide that remove in the raw material of DS-1 desulfurizing agent that at first adopt my company to produce then use the 20 cubic metres of mercaptan that transform in the raw material of desulfurizing agent that relate among the present invention, and the outlet hydrogen sulfide content is stable less than 0.1 * 10
-6, mercaptans content is stable less than 3 * 10
-6, total sulfur≤130 * 10
-6, the product copper corrosion after making with extra care is not more than 1 grade, and by doctor's experiment, foul smell removes fully, and the outlet sulphur content reaches design objective.
Embodiment 9
Taking by weighing saltpetre 10 grams, iron(ic) chloride 9 grams and nickel acetate 5 grams is dissolved in the 60 gram water, pour into then in the beaker that 100 gram absorbent charcoal carriers are housed, solution absorption is complete, taking-up is spread out and is dried 2 hours, under 120 ℃ of conditions, dried 2.5 hours then, promptly make object-desulfurizing agent in activation under 450 ℃ of nitrogen atmospheres after 4 hours at last.
With this desulfurizing agent at 30 ℃ and 5h
-1Handle the solvent oil that contains 1000mgS/L mercaptan under the air speed, outlet mercaptans content 3mgS/L is by doctor's experiment, the Sulfur capacity 14.3% (wt) of this essence desulfurization.
Claims (5)
1. the desulfurizing agent of mercaptan in the normal temperature convert liquid hydrocarbons, it is characterized in that, this desulfurizing agent is carrier with the gac, 1～3 kind of metallic compound in load iron(ic) chloride, Cobaltous diacetate, nickel acetate, cupric chloride, ammonium molybdate, zinc acetate, nitrocalcite, saltpetre, the magnesium nitrate is made, the composition of desulfurizing agent is in the carrier quality, and described 1～3 kind of metallic compound total amount of load is 10%～30% of a carrier.
2. the desulfurizing agent of mercaptan is characterized in that in the normal temperature convert liquid hydrocarbons according to claim 1, and described carrier active carbon can replace with activated alumina or molecular sieve or silica-alumina supports.
3. the preparation method of the desulfurizing agent of mercaptan in the described normal temperature convert liquid hydrocarbons of claim 1 is characterized in that, is undertaken by following steps in sequence:
1), with described metallic compound wiring solution-forming;
2), the solution that 1～3 kind of metallic compound is made into is poured in the container that carrier is housed impregnated carrier into;
3), the carrier that will flood metallic compound is spread out and is dried in the shade 2～4 hours;
4), the carrier that will dry in the shade 100～150 ℃ dry 2～4 hours down, activation promptly makes desulfurizing agent more than 3 hours under 200-500 ℃ of nitrogen atmosphere then.
4. the application of the desulfurizing agent of mercaptan in the described normal temperature convert liquid hydrocarbons of claim 1 is characterized in that, is-30～180 ℃ in temperature, and air speed is 0.01～12h
-1Under the condition, processing contains liquefied petroleum gas (LPG), solvent oil or the petroleum naphtha liquid hydrocarbon of mercaptan, and mercaptan is converted into disulphide, removes precision for mercaptan is removed to below the 5mgS/L from 1000mgS/L, liquid hydrocarbon after guaranteeing to handle is tested the Sulfur capacity 2%-15% (wt) of desulfurizing agent by doctor.
5. the application of the desulfurizing agent of mercaptan in the described normal temperature convert liquid hydrocarbons of claim 1 is characterized in that, is 0～150 ℃ in temperature, and air speed is 0.01～12h
-1Under the condition, processing contains liquefied petroleum gas (LPG), solvent oil or the petroleum naphtha liquid hydrocarbon of mercaptan, and mercaptan is converted into disulphide, removes precision for mercaptan is removed to below the 5mgS/L from 1000mgS/L, liquid hydrocarbon after guaranteeing to handle is tested the Sulfur capacity 2%-15% (wt) of desulfurizing agent by doctor.
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| CN104437496A (en) * | 2014-10-30 | 2015-03-25 | 沈阳三聚凯特催化剂有限公司 | Method for preparing desulfurizing agent |
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| CN103012032A (en) * | 2011-09-28 | 2013-04-03 | 中国石油化工股份有限公司 | Method for preparing pentane by hydrogenating light C5 fractions |
| CN104437496A (en) * | 2014-10-30 | 2015-03-25 | 沈阳三聚凯特催化剂有限公司 | Method for preparing desulfurizing agent |
| CN105126597A (en) * | 2015-07-30 | 2015-12-09 | 沈阳三聚凯特催化剂有限公司 | Refinery waste gas desulfurizer, preparation method and applications thereof |
| CN105126597B (en) * | 2015-07-30 | 2017-11-14 | 沈阳三聚凯特催化剂有限公司 | A kind of refinery off gas desulfurizing agent, its preparation method and application |
| US20190151797A1 (en) * | 2016-04-25 | 2019-05-23 | Start-Catalyst Llc | Device, process, and catalyst intended for desulfurization and demercaptanization of gaseous hydrocarbons |
| US10478773B2 (en) * | 2016-04-25 | 2019-11-19 | Start-Catalyst Llc | Device, process, and catalyst intended for desulfurization and demercaptanization of gaseous hydrocarbons |
| CN106179328A (en) * | 2016-07-08 | 2016-12-07 | 华烁科技股份有限公司 | A kind of deep purifying desulfurizing agent and preparation method thereof |
| CN106179328B (en) * | 2016-07-08 | 2019-01-04 | 华烁科技股份有限公司 | A kind of deep purifying desulfurizing agent and preparation method thereof |
| CN107774323A (en) * | 2016-08-29 | 2018-03-09 | 中国石油化工股份有限公司 | Catalyst used in natural gas production acetylene method vinyl acetate |
| CN109225137A (en) * | 2018-10-31 | 2019-01-18 | 榆林学院 | A kind of preparation method of the cobalt improved apricot shell active carbon of chlorination |
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Application publication date: 20100623 |