CN108295809B - Composite desulfurization adsorbent and preparation method and application thereof - Google Patents
Composite desulfurization adsorbent and preparation method and application thereof Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
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- C10G25/003—Specific sorbent material, not covered by C10G25/02 or C10G25/03
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
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Abstract
A composite desulfurization adsorbent and a preparation method thereof, wherein the composite desulfurization adsorbent comprises 100 parts by weight of modified mesoporous molecular sieve, 50-80 parts by weight of modified microporous molecular sieve, 20-30 parts by weight of alumina and 15-30 parts by weight of nitric acid solution; the method comprises the following steps: uniformly mixing the modified mesoporous molecular sieve, the modified microporous molecular sieve, the alumina and the nitric acid solution, extruding and forming into particles, and solidifying at room temperature; and drying the cured particles, and roasting and activating at high temperature to obtain the composite desulfurization adsorbent. The application also provides the application of the composite desulfurization adsorbent in removing sulfide in sulfur-containing substances. The composite desulfurization adsorbent can effectively remove various sulfides in sulfur-containing substances, simplifies the desulfurization process, and is simple in preparation process, easy in preparation raw material obtaining and low in cost.
Description
Technical Field
The application relates to, but is not limited to, adsorption desulfurization technology, in particular to, but not limited to, a composite desulfurization adsorbent, and a preparation method and application thereof.
Background
The carbon tetrahydrocarbon comprises components such as monoolefin (n-butene, isobutene, cis-2-butene and trans-2-butene), diolefin (butadiene), alkane (normal butane and isobutane) and the like, and is an important basic raw material of petrochemical products. The carbon tetrahydrocarbon is mainly used for producing alkylated gasoline, methyl tert-butyl ether (MTBE), methyl ethyl ketone and the like, and has wide and important application in industrial production. However, the tetracarbon generally contains sulfides such as disulfides, mercaptans, and thioethers. The existence of the sulfides can cause catalyst poisoning of a downstream deep processing technology of the carbon tetrad, influence the quality of subsequent products, cause the sulfur content of the products to exceed the standard, and cause the chemical equipment to be seriously corroded. Therefore, it is necessary to remove the sulfur compounds in the four carbon components.
Chinese patent CN101249366 discloses a refined desulfurization method for four carbon components in a refinery, which comprises the steps of firstly carrying out coarse desulfurization on four carbon components in the refinery through solid alkali, and then respectively contacting the four carbon components in the refinery after the coarse desulfurization with a carbonyl sulfur adsorbent and a refined desulfurization adsorbent to remove residual sulfides in the four carbon components. The desulfurization process can reduce the content of the sulfur compounds in the carbon four-hydrocarbon to a low level.
Disclosure of Invention
The following is a summary of the subject matter described in detail herein. This summary is not intended to limit the scope of the claims.
The inventors of the present application have found that existing carbon four desulfurization processes suffer from one or more of the following disadvantages: 1) only partial sulfide is removed; 2) the desulfurization depth is not enough, the energy consumption in the desulfurization process is large, the operation condition is harsh, and the desulfurization process is not environment-friendly; 3) because the types of sulfides in the hydrocarbon four are more, a plurality of desulfurizing agents are often needed to be matched for use, so that the desulfurizing process is more complicated, and the operation cost is high. For example, the chinese patent CN101249366 has the disadvantages of requiring the use of a plurality of desulfurizing agents, complex desulfurizing process and high operation cost.
On the basis of careful research on the existing carbon four-desulfurization method, the inventor of the application provides a composite desulfurization adsorbent with good desulfurization effect, simple desulfurization process and lower cost and a preparation method thereof.
Specifically, the application provides a composite desulfurization adsorbent, which comprises the following components in parts by weight:
in an embodiment of the present application, the modified mesoporous molecular sieve may be a mesoporous molecular sieve loaded with a metal active component, and the metal active component may be selected from any one or more of copper nitrate, cobalt nitrate, and zinc nitrate.
In an embodiment of the present application, the loading amount of the metal active component may be 10% to 40% by mass of the mesoporous molecular sieve.
Optionally, the loading amount of the metal active component can be 20-30% of the mass of the mesoporous molecular sieve.
In embodiments herein, the mesoporous molecular sieve may be selected from any one or more of MCM-41, MCM-22, MCM-48, SBA-15, and SBA-16 molecular sieves.
Optionally, the mesoporous molecular sieve may be selected from any one or more of MCM-41, MCM-48 and SBA-15 molecular sieves.
In an embodiment of the present application, the specific surface area of the modified mesoporous molecular sieve may be 600 to 1250m2/g。
In an embodiment of the present application, the modified microporous molecular sieve may be a 13X molecular sieve modified by an ion exchange method using a metal salt solution, and the metal salt may be any one selected from the group consisting of cerium nitrate-manganese nitrate, cerium nitrate-nickel nitrate, and cerium nitrate-manganese nitrate-nickel nitrate.
Optionally, the concentration of nitrate ions in the metal salt solution can be 0.1-0.3 mol/L.
In an embodiment of the present application, the alumina may be γ -Al2O3。
In an embodiment of the present application, the alumina may have a specific surface area of 230 to 300m2/g。
In the present application, the nitric acid solution mainly plays a role of binding, and thus the mass fraction thereof has substantially no influence on the desulfurization effect. In an embodiment of the present application, the mass fraction of the nitric acid solution may be 5 to 10%.
The application also discloses a method for preparing the composite desulfurization adsorbent, which comprises the following steps:
uniformly mixing the modified mesoporous molecular sieve, the modified microporous molecular sieve, the alumina and the nitric acid solution, extruding and forming into particles, and solidifying at room temperature;
and drying the cured particles, and roasting and activating at high temperature to obtain the composite desulfurization adsorbent.
In an embodiment of the present invention, the high-temperature baking may be performed at a temperature of 400 to 550 ℃ for 5 to 8 hours.
In an embodiment of the present application, the temperature for drying the particles may be 80 to 120 ℃ and the time may be 5 to 12 hours.
In an embodiment of the present application, the curing time may be 0.5 to 1 hour.
In an embodiment of the present application, the modified mesoporous molecular sieve may be obtained by: loading the metal active component on the mesoporous molecular sieve by an isometric impregnation method, and drying to obtain the modified mesoporous molecular sieve.
In the embodiment of the application, the temperature for drying the modified mesoporous molecular sieve can be 80-120 ℃, and the time can be 5-12 h.
In embodiments of the present application, the modified microporous molecular sieve may be obtained by: and modifying the microporous molecular sieve by using a metal salt solution by adopting an ion exchange method, and drying after ion exchange to obtain the modified microporous molecular sieve.
In the embodiment of the present application, the time of the ion exchange may be 12 to 24 hours.
In the embodiment of the present application, the temperature for drying the modified microporous molecular sieve may be 80 to 120 ℃ and the time may be 5 to 12 hours.
The application also provides the application of the composite desulfurization adsorbent as described above in removing sulfide in sulfur-containing substances.
In embodiments herein, the sulfur species may be a tetracarbon.
Compared with the prior art, the composite desulfurization adsorbent and the preparation method thereof have the following advantages:
(1) the modified mesoporous molecular sieve and the modified microporous molecular sieve are compounded, the desulfurization performance of the modified mesoporous molecular sieve and the desulfurization performance of the modified microporous molecular sieve are integrated, the modified mesoporous molecular sieve and the modified microporous molecular sieve form complementary functions, and the advantages of different sulfides can be exerted respectively. The modified microporous molecular sieve has a good removal effect on most sulfides, but the desulfurization effect on part of macromolecular sulfides is poor due to the small pore diameter of the modified microporous molecular sieve. The introduction of the modified mesoporous molecular sieve can effectively make up for the defect, and the modified mesoporous molecular sieve has larger specific surface area and pore volume, so that the desulfurization performance of the composite desulfurization adsorbent is further improved.
(2) The modified mesoporous molecular sieve and the modified microporous molecular sieve in the composite desulfurization adsorbent have different desulfurization active components, and the coexistence of the different active components produces a synergistic effect, so that the composite desulfurization adsorbent can effectively remove sulfides in sulfur-containing substances.
(3) In order to solve the problem, alumina is introduced in the process of preparing the composite desulfurization adsorbent, the alumina plays a role in forming a binder on one hand, and has a desulfurization effect on the other hand, so that the influence caused by partial loss of the active component is overcome.
(4) The composite desulfurization adsorbent has the advantages of simple preparation process, easily obtained preparation raw materials and low cost, and can effectively remove various sulfides, so that the composite desulfurization adsorbent is not required to be matched with other desulfurizing agents for use, and the desulfurization process is simplified.
Additional features and advantages of the application will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the application. The objectives and other advantages of the application may be realized and attained by the structure particularly pointed out in the written description and claims hereof.
Detailed Description
Hereinafter, embodiments of the present application will be described in detail to make objects, technical solutions and advantages of the present application more apparent. It should be noted that the embodiments and features of the embodiments in the present application may be arbitrarily combined with each other without conflict.
The raw materials and reagents used in the following examples are all common commercial products unless otherwise specified.
Example 1
The composite desulfurization adsorbent of the present example was prepared by the following method:
(1) loading metal active component copper nitrate on MCM-41 mesoporous molecular sieve (specific surface area is 1000 m) by adopting an isometric impregnation method2And/g), wherein the loading amount of the copper nitrate is 30% of the mass of the mesoporous molecular sieve, and the modified mesoporous molecular sieve is obtained after the copper nitrate is loaded and dried in an oven at 120 ℃ for 6 hours.
(2) Modifying a 13X molecular sieve by using a cerous nitrate-manganese nitrate-nickel nitrate metal salt solution (the concentration of nitrate ions is 0.3mol/L) by adopting an ion exchange method, carrying out ion exchange for 24 hours, and drying in an oven at 120 ℃ for 6 hours to obtain the modified microporous molecular sieve.
(3) 100 parts by weight of the modified mesoporous molecular sieve obtained above, 80 parts by weight of the modified microporous molecular sieve, and 30 parts by weight of alumina (specific surface area 300 m)2And the weight portions of nitric acid solution (the mass fraction is 8 percent) and 30 weight portions of nitric acid solution are uniformly mixed, extruded and molded to obtain cylindrical particles, and the cylindrical particles are solidified for 1 hour at room temperature.
(4) And (3) placing the cylindrical particles in a drying oven, drying at 120 ℃ for 6h, then placing in a muffle furnace, and roasting and activating at 550 ℃ for 5h to obtain the formed carbon-tetrahydrocarbon composite desulfurization adsorbent.
Example 2
The composite desulfurization adsorbent of the present example was prepared by the following method:
(1) loading metal active component cobalt nitrate on MCM-48 mesoporous molecular sieve (specific surface area is 800 m) by adopting an isometric impregnation method2Per g) whereinThe loading capacity of the cobalt nitrate is 25% of the mass of the mesoporous molecular sieve, and the supported cobalt nitrate is dried in an oven at 100 ℃ for 8 hours to obtain the modified mesoporous molecular sieve.
(2) Modifying a 13X molecular sieve by using a cerous nitrate-manganese nitrate metal salt solution (the concentration of nitrate ions is 0.2mol/L) by adopting an ion exchange method, and drying the modified microporous molecular sieve in an oven at 100 ℃ for 8 hours after ion exchange for 18 hours to obtain the modified microporous molecular sieve.
(3) 100 parts by weight of the modified mesoporous molecular sieve obtained above, 70 parts by weight of the modified microporous molecular sieve, and 20 parts by weight of alumina (specific surface area 300 m)2And the weight portions of nitric acid solution (the mass fraction is 7 percent) and are uniformly mixed, and then the mixture is extruded and formed to obtain cylindrical particles which are solidified for 1 hour at room temperature.
(4) And (3) placing the cylindrical particles in a drying oven, drying for 8h at 100 ℃, then placing in a muffle furnace for roasting and activating at 500 ℃ for 7h to obtain the formed carbon-tetrahydrocarbon composite desulfurization adsorbent.
Example 3
The composite desulfurization adsorbent of the present example was prepared by the following method:
(1) loading a metal active component zinc nitrate on an SBA-15 mesoporous molecular sieve (the specific surface area is 1100 m) by adopting an isometric impregnation method2And/g), wherein the loading amount of the zinc nitrate is 20% of the mass of the mesoporous molecular sieve, and the modified mesoporous molecular sieve is obtained after the zinc nitrate is loaded and dried in an oven at 90 ℃ for 12 hours.
(2) Modifying a 13X molecular sieve by using a cerous nitrate-nickel nitrate metal salt solution (the concentration of nitrate ions is 0.1mol/L) by adopting an ion exchange method, and drying the modified microporous molecular sieve in an oven at 90 ℃ for 12 hours after ion exchange for 12 hours to obtain the modified microporous molecular sieve.
(3) Weighing 100 parts by weight of modified mesoporous molecular sieve, 60 parts by weight of modified microporous molecular sieve and 20 parts by weight of alumina (the specific surface area is 260 m)2And the weight portions of nitric acid solution (the mass fraction is 7 percent) and are uniformly mixed, and then the mixture is extruded and formed to obtain cylindrical particles, and the cylindrical particles are solidified for 0.5 hour at room temperature.
(4) And (3) placing the cylindrical particles in a drying oven, drying for 12h at 90 ℃, and then placing in a muffle furnace for roasting and activating at 450 ℃ for 8h to obtain the formed carbon-tetrahydrocarbon composite desulfurization adsorbent.
Comparative example 1
The desulfurization adsorbent of the embodiment is a modified mesoporous molecular sieve, which is prepared by the following method:
loading metal active component copper nitrate on MCM-41 mesoporous molecular sieve (specific surface area is 1000 m) by adopting an isometric impregnation method2And/g), wherein the loading amount of the copper nitrate is 30% of the mass of the mesoporous molecular sieve, and the modified mesoporous molecular sieve is obtained after the copper nitrate is loaded and dried in an oven at 120 ℃ for 6 hours.
Comparative example 2
The desulfurization adsorbent of the present example is a modified microporous molecular sieve, which is prepared by the following method:
modifying a 13X molecular sieve by using a cerous nitrate-manganese nitrate-nickel nitrate metal salt solution (the concentration of nitrate ions is 0.3mol/L) by adopting an ion exchange method, carrying out ion exchange for 24 hours, and drying in an oven at 120 ℃ for 6 hours to obtain the modified microporous molecular sieve.
Test example
The desulfurization effects of the desulfurization adsorbents of the above examples 1 to 3 and comparative examples 1 to 2 were tested, and the results are shown in table 1. Wherein the adsorption temperature is 30 ℃, the pressure is 1.2Mpa, and the space velocity of the carbon-tetrad hydrocarbon raw material is 1.5h-1。
TABLE 1 Sulfur content before and after carbon tetracarbon treatment with desulfurizing adsorbent
| Carbon four hydrocarbon feedstock | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | |
| Sulfur content (μ g/g) | 300 | 1.5 | 2 | 5 | 32 | 21 |
As can be seen from table 1, the composite desulfurization adsorbents in embodiments 1 to 3 of the present application can effectively remove sulfides in hydrocarbons, and the desulfurization effect is significantly better than that of a single modified mesoporous molecular sieve or a single modified microporous molecular sieve, which means that after the composite desulfurization adsorbent of the present application compounds the modified mesoporous molecular sieve and the modified microporous molecular sieve, the modified mesoporous molecular sieve and the modified microporous molecular sieve form complementary functions, and can exert advantages on different sulfides. Moreover, after the composition, a synergistic effect is obtained, because the modified mesoporous molecular sieve and the modified microporous molecular sieve have different active components, and the existence of different metal active components has a synergistic effect.
Although the embodiments disclosed in the present application are described above, the descriptions are only for the convenience of understanding the present application, and are not intended to limit the present application. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the disclosure as defined by the appended claims.
Claims (11)
1. The composite desulfurization adsorbent comprises the following components in parts by weight:
the modified mesoporous molecular sieve is a mesoporous molecular sieve loaded with metal active components, and the metal active components are selected from any one or more of copper nitrate, cobalt nitrate and zinc nitrate;
the loading amount of the metal active component is 10-40% of the mass of the mesoporous molecular sieve;
the mesoporous molecular sieve is selected from any one or more of MCM-41, MCM-22, MCM-48, SBA-15 and SBA-16 molecular sieves;
the modified microporous molecular sieve is a 13X molecular sieve obtained by modifying a metal salt solution by an ion exchange method, wherein the metal salt is selected from any one of cerium nitrate-manganese nitrate, cerium nitrate-nickel nitrate and cerium nitrate-manganese nitrate-nickel nitrate;
the concentration of nitrate ions in the metal salt solution is 0.1-0.3 mol/L.
2. The composite desulfurization adsorbent according to claim 1, wherein the specific surface area of the modified mesoporous molecular sieve is 600 to 1250m2/g。
3. The composite desulfurization adsorbent according to claim 1, wherein the loading amount of the metal active component is 20 to 30% by mass of the mesoporous molecular sieve.
4. The composite desulfurization adsorbent of claim 1, wherein the mesoporous molecular sieve is selected from any one or more of MCM-41, MCM-48, and SBA-15 molecular sieves.
5. The composite desulfurization sorbent of claim 1, wherein the alumina is γ -Al2O3(ii) a The specific surface area of the alumina is 230-300 m2/g。
6. A method of preparing the composite desulfurization sorbent of any one of claims 1-5, comprising the steps of:
uniformly mixing the modified mesoporous molecular sieve, the modified microporous molecular sieve, the alumina and the nitric acid solution, extruding and forming into particles, and solidifying at room temperature;
and drying the cured particles, and roasting and activating at high temperature to obtain the composite desulfurization adsorbent.
7. The method of claim 6, wherein the high-temperature roasting temperature is 400-550 ℃ and the time is 5-8 h.
8. A process according to claim 6, wherein the temperature for drying the particles is from 80 to 120 ℃ for from 5 to 12 hours; optionally, the curing time is 0.5-1 h.
9. The process according to any one of claims 6-8, wherein the modified mesoporous molecular sieve is obtained by: loading the metal active component on the mesoporous molecular sieve by adopting an isometric impregnation method, and drying to obtain the modified mesoporous molecular sieve;
the drying temperature of the modified mesoporous molecular sieve is 80-120 ℃, and the drying time is 5-12 h.
10. The process of any of claims 6-8, wherein the modified microporous molecular sieve is obtained by: modifying the microporous molecular sieve by using a metal salt solution by adopting an ion exchange method, and drying after ion exchange to obtain the modified microporous molecular sieve;
the time of the ion exchange is 12-24 h;
the temperature for drying the modified microporous molecular sieve is 80-120 ℃, and the time is 5-12 h.
11. Use of the composite desulfurization adsorbent according to any one of claims 1 to 5 for removing sulfide from sulfur-containing substances; the sulfur species is a carbon tetrahydrocarbon.
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