CN101590395A - A kind of preparation method of load-type desulfurizer - Google Patents
A kind of preparation method of load-type desulfurizer Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of load-type desulfurizer, may further comprise the steps: the 1. activation of carrier; 2. active metallic compound is dissolved in and is mixed with maceration extract in the solvent; 3. with step 1. in activation back carrier impregnation in the described maceration extract that step obtains in 2., through filtering, obtaining the carrier that load has active metallic compound after the drying; 4. step is obtained carrier impregnation that described load has active metallic compound in 3. in inorganic alkaline solution, through filtration, drying, obtain the desulfurizing agent finished product through after the roasting again.The desulfurizing agent that obtains by the preparation method among the present invention has active component decentralization height, advantage that load capacity is big, thereby has high desulfurization rate.
Description
Technical field
The invention belongs to the desulfurizing agent field, particularly relate to a kind of preparation method of load-type desulfurizer that is used for removing various oil product sulfide.
Background technology
Along with constantly the carrying out of oil extraction, sulfur content is the trend that rises year by year in the oil product in recent years, and people must improve constantly the needs that the desulphurizing ability of desulfurizing agent could satisfy further production or process.The method that now prepares desulfurizing agent mainly comprises kneading method and infusion process two big classes, and than adopting pure mechanical kneading method to prepare the kneading method of desulfurizing agent, active component has higher decentralization in the desulfurizing agent that immersion process for preparing goes out.
Chinese patent CN1609171 discloses a kind of preparation method of desulfurizing agent, this desulfurizing agent with the alumina mixture of Different Pore Structures as carrier, earlier with the aqueous solution oxide impregnation alumina supporter that contains alkaline assistant, contain the desulfurizing agent of alkaline assistant after drying, the roasting again with the aqueous solution dipping that contains active metallic compound, obtain the desulfurizing agent finished product after drying, the roasting again.The defective that exists in the prior art is:
1) at first alkaline matter is carried on the carrier in the prior art, the carrier impregnation that will contain alkaline matter again is in the aqueous solution that contains active metallic compound, this moment, metal ion can generate the metal hydroxides of poorly water-soluble with alkaline matter, these materials are attached to the carrier outer surface and are difficult to enter into the pore passage structure of carrier again, make dispersion degree of active components and load capacity reduce greatly, cause Sulfur capacity not high.
2) in the prior art, because deliquescent restriction, usually active metallic compound is dissolved in the water, the power that active metallic compound is distributed to the carrier inner surface only is the concentration difference of carrier surfaces externally and internally solution, mode by capillarity and diffusion loads on the carrier, therefore load capacity and the decentralization at carrier inner surface active metallic compound can be restricted, thereby causes desulfurized effect undesirable.In addition, owing to adopt twice high-temperature calcination process in the prior art, so the consumption of the energy is bigger.
Summary of the invention
For this reason, technical problem to be solved by this invention is: overcome the defective that the active component decentralization is low in the desulfurizing agent in the prior art, load capacity is little, a kind of active component decentralization height, preparation method of load-type desulfurizer that load capacity is big are provided.
For solving the problems of the technologies described above, the invention provides a kind of preparation method of load-type desulfurizer and may further comprise the steps: the 1. activation of carrier; 2. active metallic compound is dissolved in and is mixed with maceration extract in the solvent; 3. with step 1. in activation back carrier impregnation in the described maceration extract that step obtains in 2., through filtering, obtaining the carrier that load has active metallic compound after the drying; 4. step is obtained carrier impregnation that described load has active metallic compound in 3. in inorganic alkaline solution, through filtration, drying, obtain the desulfurizing agent finished product through after the roasting again.
Step 1. in, the temperature of activation process is 120-350 ℃, the time is 8-36 hour.Described carrier is each molecular sieve analog, alundum (Al, active carbon, carbon fiber, modenite or high aluminosilicate.
Step 2. in, described solvent is the mixed liquor that one or both and the organic solvent in water, the 3-28wt% ammoniacal liquor forms.Described organic solvent is methyl-sulfoxide, ethylene glycol, methyl alcohol, N, one or more in dinethylformamide, the ethanol.
Step 3. in, the baking temperature of dry run is 80-180 ℃, be 5-10 hour drying time.Dip time is 6-48 hour.
Step 4. in, described inorganic alkaline solution is NaOH and/or potassium hydroxide solution.Dip time is 6-24 hour.The baking temperature of dry run is 80-180 ℃, and be 5-10 hour drying time; The sintering temperature of roasting process is 180-480 ℃, and roasting time is 5-10 hour.
Described active metallic compound is one or more in the water soluble salt of iron, copper, zinc, nickel, calcium, magnesium.
Compared with prior art the present invention has following advantage:
1) owing to earlier active metallic compound is carried on the carrier among the present invention, and then the carrier of active metallic compound arranged with inorganic alkali lye dip loading, therefore avoid metal ion and alkali lye generation to be difficult for molten metal hydroxides and only be attached to carrier surface and be difficult to enter defective in the carrier duct, improved the decentralization and the load capacity of active metallic compound greatly.
2) among the present invention active metallic compound is dissolved in the organic and inorganic mixed solvent, because organic solvent has the effect that reduces solution polarity and viscosity, therefore in dipping process, help active component to be scattered in the inner surface of carrier, can not cause active metallic compound only to adsorb at the carrier outer surface, only generate the metal hydroxides of deposition in the time of can avoiding again steeping liquor, thereby further improve decentralization and the load capacity of active component on carrier in the reaction of carrier outer surface.Only in the end adopt high-temperature calcination process in the step among the present invention in addition, saved energy consumption to greatest extent.
The specific embodiment
At first preparation method of load-type desulfurizer among the present invention is described further.Preparation method of the present invention can be divided into: the carrier activation, and the maceration extract preparation, load has the preparation of active metallic compound carrier, and alkali lye is handled.
The carrier activation
Carriers such as each molecular sieve analog, alundum (Al, active carbon, carbon fiber, modenite, high aluminosilicate at 120-350 ℃ of following heat treated 8-36 hour, are finished activation process.The non-emphasis of the present invention of this step and being well known to those skilled in the art is not so give unnecessary details.
The maceration extract preparation
Active metallic compound is dissolved in and is mixed with solution in the solvent, promptly is used for the maceration extract of impregnated carrier.The solvent of preparation maceration extract is the mixed solvent of one or both and organic solvent in water, the 3-28wt% ammoniacal liquor among the present invention.Owing to contained organic solvent in the maceration extract, make easier the entering in the carrier duct of active component, better be scattered on the carrier inner surface, improved load capacity and the decentralization of reactive metal on carrier, thereby can improve the desulfurized effect of desulfurizing agent greatly, main cause is: on the one hand, organic solvent can play the effect that reduces the viscosity that contains the active metallic compound maceration extract, and maceration extract is also with regard in the carrier duct, easier immersion road; On the other hand, because the polarity of organic solvent is little, volatile, the organic solvent in the duct can impel being carried on the carrier inner surface that active component disperses more in the process of volatilization fast, thereby has improved dispersion degree of active components.
Adopt the organic solvent with certain polarity among the present invention, as methyl-sulfoxide, ethylene glycol, methyl alcohol, N, one or more in dinethylformamide, the ethanol can better mix with inorganic solvent so mutually.
Active metallic compound is one or more in the water soluble salt of iron, copper, zinc, nickel, calcium, magnesium, as the chloride of iron, copper, zinc, nickel, calcium, magnesium, nitrate, sulfate etc.
Load has the preparation of active metallic compound carrier
In the solution for preparing, the preferred 6-48 of dip time hour, dipping process can reach balance substantially in this time range, promptly finishes dipping process with the carrier impregnation after the activation.After finishing dipping, carrier is filtered out from maceration extract, obtained the carrier that load has active metallic compound after under 80-180 ℃ dry 5-10 hour, wherein, active metallic compound accounts for the 2-10% of dipping, dried total weight of carrier.
Alkali lye is handled
The carrier impregnation that load is had active metallic compound floods that dipping process can reach balance after 6-24 hour in inorganic alkaline solution.Soaked carrier is filtered out from alkali lye, after under 80-180 ℃ dry 5-10 hour, can obtain final desulfurizing agent finished product at 180-480 ℃ of following roasting 5-10 hour again.Adopt the purpose of the carrier of inorganic alkali lye dip loading active component to be among the present invention: metallic compound in the carrier duct and alkali react and partly or entirely generate metal hydroxides, decomposition reaction takes place in these hydroxide that are carried on the carrier inner surface when roasting, partially or completely generate reactive metal oxides, the particle diameter of these metallic compounds is several nanometers between tens nanometers and be dispersed in uniformly in the carrier duct, therefore in the desulfurizing agent finished product of the present invention's preparation on the carrier active component of load exist with the form of metal oxide or metal hydroxides, than metallic salt, the metallic compound of these two kinds of forms all has good desulfurized effect.
NaOH that the alkaline solution that adopts among the present invention preferably is easy to get and/or potassium hydroxide solution, the preferred 5-30wt% of solution concentration.
Next describe by the performance of specific embodiment preparation method by desulfurizing agent among the present invention and the desulfurizing agent that obtains.
Embodiment 1 preparation desulfurizing agent C1
1. with alumina carrier 350 ℃ of following heat treated 30 hours.
2. zinc chloride and zinc nitrate mixture are dissolved in water and N, and the dinethylformamide volume ratio is to be mixed with maceration extract in 8: 1 the solvent.
3. the carrier impregnation after will activating was flooded 48 hours in the maceration extract for preparing, and carrier is filtered out from maceration extract, obtained the carrier that load has zinc chloride and zinc nitrate after under 180 ℃ dry 5 hours, and wherein the content of zinc chloride and zinc nitrate is 2wt%.
4. the carrier impregnation that load is had zinc chloride and zinc nitrate was flooded 6 hours in the 30wt% potassium hydroxide solution, and soaked carrier is filtered out from alkali lye, after under 180 ℃ dry 5 hours, obtained desulfurizing agent C1 in 5 hours 480 ℃ of following roastings again.The desulfurization performance of C1 sees Table 1.
Embodiment 2 preparation desulfurizing agent C2
1. with the mixed carrier of high aluminosilicate and active carbon 120 ℃ of following heat treated 36 hours.
2. to be dissolved in 3wt% ammoniacal liquor and ethylene glycol volume ratio be to be mixed with maceration extract in 10: 1 the solvent for iron chloride and copper nitrate mixture.
3. the carrier impregnation after will activating was flooded 24 hours in the maceration extract for preparing, and carrier is filtered out from maceration extract, obtained the carrier that load has iron chloride and copper nitrate after under 80 ℃ dry 10 hours, and wherein the content of iron chloride and copper nitrate is 10wt%.
4. the carrier impregnation that load is had iron chloride and copper nitrate was flooded 24 hours in the 5wt% sodium hydroxide solution, and soaked carrier is filtered out from alkali lye, after under 80 ℃ dry 10 hours, obtained desulfurizing agent C2 in 10 hours 180 ℃ of following roastings again.The desulfurization performance of C2 sees Table 1.
Embodiment 3 preparation desulfurizing agent C3
1. with carbon fibre carrier 180 ℃ of following heat treated 8 hours.
2. to be dissolved in water and methyl-sulfoxide volume ratio be to be mixed with maceration extract in 8: 1 the solvent to the mixture of calcium chloride and magnesium chloride.
3. the carrier impregnation after will activating was flooded 6 hours in the maceration extract for preparing, and carrier is filtered out from maceration extract, obtained the carrier that load has calcium chloride and magnesium chloride after under 120 ℃ dry 7 hours, and wherein the content of calcium chloride and magnesium chloride is 8wt%.The desulfurization performance of C3 sees Table 1.
4. the carrier impregnation that load is had calcium chloride and magnesium nitrate is in the mixed solution of 15wt% NaOH and potassium hydroxide, flooded 18 hours, soaked carrier is filtered out from alkali lye, after under 180 ℃ dry 8 hours, obtained desulfurizing agent C3 in 8 hours 200 ℃ of following roastings again.The desulfurization performance of C3 sees Table 1.
Embodiment 4 preparation desulfurizing agent C4
1. with the ZSM-5 molecular sieve carrier 200 ℃ of following heat treated 24 hours.
2. to be dissolved in 10wt% ammoniacal liquor, water, methyl-sulfoxide volume ratio be to be mixed with maceration extract in 2: 8: 1 the solvent for nickel nitrate, ferric nitrate, zinc nitrate.
3. the carrier impregnation after will activating was flooded 12 hours in the maceration extract for preparing, carrier is filtered out from maceration extract, obtained the carrier that load has nickel nitrate, ferric nitrate, zinc nitrate after under 120 ℃ dry 8 hours, wherein the content of nickel nitrate, ferric nitrate, zinc nitrate is 10wt%.
4. the carrier impregnation that load is had nickel nitrate, ferric nitrate, zinc nitrate is in the 20wt% sodium hydroxide solution, flooded 12 hours, soaked carrier is filtered out from alkali lye, after under 120 ℃ dry 8 hours, obtained desulfurizing agent C4 in 7 hours 300 ℃ of following roastings again.The desulfurization performance of C4 sees Table 1.
Embodiment 5 preparation desulfurizing agent C5
1. with the modenite carrier 250 ℃ of following heat treated 30 hours.
2. copper sulphate, magnesium chloride, calcium chloride mixture are dissolved in the mixed liquor of ethanol/methyl alcohol and the solvent that water volume ratio is 1: 8 and are mixed with maceration extract.
3. the carrier impregnation after will activating was flooded 36 hours in the maceration extract for preparing, carrier is filtered out from maceration extract, obtained the carrier that load has copper sulphate, magnesium chloride, calcium chloride after under 120 ℃ dry 8 hours, wherein the content of copper sulphate, magnesium chloride, calcium chloride is 8wt%.
4. the carrier impregnation that load is had copper sulphate, magnesium chloride, calcium chloride is in the 20wt% potassium hydroxide solution, flooded 12 hours, soaked carrier is filtered out from alkali lye, after under 120 ℃ dry 8 hours, obtained desulfurizing agent C5 in 6 hours 350 ℃ of following roastings again.The desulfurization performance of C5 sees Table 1.
Embodiment 6 preparation desulfurizing agent C6
1. with alumina support 250 ℃ of following heat treated 36 hours.
2. nickel nitrate is dissolved in 5wt% ammoniacal liquor and N, and the dinethylformamide volume ratio is to be mixed with maceration extract in 10: 1 the solvent.
3. the carrier impregnation after will activating was flooded 18 hours in the maceration extract for preparing, and carrier is filtered out from maceration extract, obtained the carrier that load has nickel nitrate after under 120 ℃ dry 8 hours, and wherein the content of nickel nitrate is 4wt%.
4. the carrier impregnation that load is had nickel nitrate was flooded 20 hours in the 10wt% sodium hydroxide solution, and soaked carrier is filtered out from alkali lye, after under 120 ℃ dry 9 hours, obtained desulfurizing agent C6 in 6 hours 400 ℃ of following roastings again.The desulfurization performance of C6 sees Table 1.
By verifying the desulfurization performance of the desulfurizing agent C1-C6 that example investigation embodiment 1-6 prepares, the desulfurization degree method of testing is: with benzinum (90-120 ℃) is solvent, and the preparation sulfur content is the petroleum ether solution of the hydrogen sulfide of 500 μ g/g.Getting the 1g desulfurizing agent joins in the above-mentioned 50mL oil sample, under room temperature (20 ℃), airtight, electromagnetic agitation (350rpm) condition respectively the assaying reaction time be 1 hour and 2 hours after sulfur content in the oil sample, calculate the desulfurization degree of desulfurizing agent to this sulfide, wherein the computing formula of desulfurization degree is: total sulfur content * 100% in (in the oil sample after total sulfur content-desulfurization in the oil sample sulfur content)/oil sample.
Table 1
| Desulfurizing agent | React desulfurization degree/% after 1 hour | React desulfurization degree/% after 2 hours |
| C1 | 96.1 | 100 |
| C2 | 95.2 | 99.8 |
| C3 | 95.6 | 99.9 |
| C4 | 95.9 | 100 |
| C5 | 95.7 | 99.9 |
| C6 | 96.0 | 100 |
By embodiment as can be seen, the desulfurizing agent that obtains of the preparation method among the present invention can obtain than high desulfurization rate in the short period of time.
Obviously, the foregoing description only is for example clearly is described, and is not the qualification to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here need not also can't give exhaustive to all embodiments.And conspicuous variation of being extended out thus or change still are among the protection domain of claim of the present invention.
Claims (10)
1, a kind of preparation method of load-type desulfurizer may further comprise the steps:
1. the activation of carrier;
2. active metallic compound is dissolved in and is mixed with maceration extract in the solvent;
3. with step 1. in activation back carrier impregnation in the described maceration extract that step obtains in 2., through filtering, obtaining the carrier that load has active metallic compound after the drying;
4. step is obtained carrier impregnation that described load has active metallic compound in 3. in inorganic alkaline solution, through filtration, drying, obtain the desulfurizing agent finished product through after the roasting again.
2, preparation method of load-type desulfurizer according to claim 1 is characterized in that: step 2. in, described solvent is the mixed liquor that one or both and the organic solvent in water, the 3-28wt% ammoniacal liquor forms.
3, preparation method of load-type desulfurizer according to claim 2 is characterized in that: step 2. in, described organic solvent is methyl-sulfoxide, ethylene glycol, methyl alcohol, ethanol, N, one or more in the dinethylformamide.
4, preparation method of load-type desulfurizer according to claim 1 is characterized in that: described active metallic compound is one or more in the water soluble salt of iron, copper, zinc, nickel, calcium, magnesium.
5, preparation method of load-type desulfurizer according to claim 1 is characterized in that: step 4. in, described inorganic alkaline solution is NaOH and/or potassium hydroxide solution.
6, preparation method of load-type desulfurizer according to claim 1 is characterized in that: the step 1. temperature of middle activation process is 120-350 ℃, and the time is 8-36 hour.
7, preparation method of load-type desulfurizer according to claim 1 is characterized in that: step 1. in, described carrier is each molecular sieve analog, alundum (Al, active carbon, carbon fiber, modenite or high aluminosilicate.
8, preparation method of load-type desulfurizer according to claim 1 is characterized in that: the step 4. sintering temperature of middle roasting process is 180-480 ℃, and roasting time is 5-10 hour.
9, preparation method of load-type desulfurizer according to claim 1 is characterized in that: step 3., 4. the baking temperature of middle dry run is 80-180 ℃, and be 5-10 hour drying time.
10, preparation method of load-type desulfurizer according to claim 1 is characterized in that: the 3. middle dip time of step is 6-48 hour, and the 4. middle dip time of step is 6-24 hour.
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| CN101590395B (en) | 2012-07-25 |
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