CN1324915A - Catalyst for converting mercaptan contained in hydrocarbon oil - Google Patents
Catalyst for converting mercaptan contained in hydrocarbon oil Download PDFInfo
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- CN1324915A CN1324915A CN 00107681 CN00107681A CN1324915A CN 1324915 A CN1324915 A CN 1324915A CN 00107681 CN00107681 CN 00107681 CN 00107681 A CN00107681 A CN 00107681A CN 1324915 A CN1324915 A CN 1324915A
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Abstract
The present invention relates to a catalyst for converting thioalcohol contained in hydrocarbon oil, and a catalyst using spinel type oxide as active component for converting thioalcohol in hydrocarbon oil. Said catalyst possesses the characteristics of quick speed for converting thioalcohol, good effect, long service life, no discharge of alkali liquor, having no need of activating agent, and convenient regeneration. It not only can completely convert thioalcohol contained in light oil, but also can use dissolved oxygen of liquefied petroleum gas to completely convert the thioalcohol in liquefied petroleum gas.
Description
The present invention relates to a catalyst for treating hydrocarbon oil including liquefied petroleum gas, naphtha, gasoline, aviation kerosene, kerosene and diesel oil.
In the process of petroleum refining, hydrocarbon oils (also called oil products) such as liquefied petroleum gas, naphtha, catalytic gasoline, straight-run aviation kerosene, lamp oil, diesel oil and the like subjected to alkali cleaning all contain a certain amount of mercaptan, are strong in corrosivity and have large odor, and are not beneficial to storage and use of materials. Mercaptan can cause the corrosion test of liquefied petroleum gas to be unqualified, so that doctor tests of gasoline and aviation kerosene cannot pass, and the quality of products is reduced or the products cannot be qualified and delivered.
The process for converting mercaptan is proposed by American Global oil products company (UOP) in 1958, and through the development of more than forty years, the technology is continuously improved, from the alkali deodorization method to the latest alkali-free deodorization method, several thousand sets of such devices are in operation in the world, the current process for converting mercaptan comprises ① liquid-liquid extraction and regeneration process, the process is suitable for the sweetening of liquefied petroleum gas or light oil products, the most basic process of the process is that after the sodium hydroxide solution dissolves poly-phthalocyanine cobalt or a sulfonated-phthalocyanine cobalt catalyst, the mixture is fully mixed and reacted with the liquefied petroleum gas or the light oil products (including naphtha, catalytic gasoline, straight-run aviation kerosene, lamp oil and diesel oil) in a tower or a container, and the mercaptan in the oil products is reacted with the sodium hydroxide to generate sodium mercaptan which enters into alkali liquor, the reaction formula is as follows:
The invention aims to provide a catalyst which has higher use efficiency, no alkali liquor discharge and no need of an activating agent and is used for converting mercaptan contained in hydrocarbon oil.
The technical scheme for realizing the purpose of the invention is as follows: the active component of the catalyst for converting mercaptan contained in hydrocarbon oil is spinel type oxide.
The general formula of the spinel-type oxide is:
(AXA’1-X)(BYB’1-Y)2O4wherein A, A 'is respectively a metal element selected from Zn, Co, Ni, Mg, Mn, Cu and Cd, B is a metal element Fe, B' is a metal element selected from Cr, Co, Ni and Mn, X is more than or equal to 0 and less than or equal to 1, Y is more than or equal to 0.4 and less than or equal to 1.0, and the active component is directly loaded on mullite, cordierite, magnesia-alumina spinel or α -Al2O3On a carrier as the main phase.
Preferred A, A' are each a metal element selected from Zn, Co, Mn; b' is metal element Cr.
The preferred active component spinel-type oxide has the formula (Zn)0.8Co0.2)(Fe0.5Cr0.5)2O4、(Zn0.6Mg0.4)(Fe0.6Cr0.4)2O4、(Zn0.5Ni0.5)(Fe0.7Cr0.3)2O4、(Zn0.7Co0.3)Fe2O4、(Zn0.5Mn0.5)(Fe0.8Cr0.2)2O4、(Zn0.5Cu0.5)(Fe0.8Cr0.2)2O4Or (Zn)0.5Cd0.5)(Fe0.8Cr0.2)2O4。
The carrier of the preferred catalyst is a carrier taking cordierite or magnesia-alumina spinel as a main phase, and the weight percentage of the main phase in the carrier is more than or equal to 80 percent.
The loading amount of the active component on the carrier is 5-15% (weight).
The catalyst with spinel type oxide as active component is used in converting mercaptan in hydrocarbon oil.
The catalyst with spinel type oxide as active component is used in converting mercaptan in liquefied petroleum gas, naphtha, gasoline, aviation kerosene, lamp oil or diesel oil.
The invention has the positive effects that: (1) crystallization chemistry to classify spinel oxides into AB2O4Compound of type (A), spinel type oxide (A) as active ingredient of catalyst of the inventionXA’1-X)(BYB’1-Y)2O4The structure belongs to AB2O4A compound of the formula (I). When the catalyst is used for converting mercaptan contained in hydrocarbon oil such as liquefied petroleum gas, naphtha, gasoline, aviation kerosene, lamp oil, diesel oil and the like, under the condition that the mercaptan in the hydrocarbon oil exists in oxygen, the mercaptan of the mercaptan is oxidized under the bridge action of electron transfer of the catalyst, the valence bond between the sulfur in the mercaptan and hydrogen is broken, and the hydrogen and the oxygen are combined to generate the mercaptanThe remaining part of the two thiol molecules is combined into a disulfide molecule, thereby achieving the purpose of converting thiol. (2) When the catalyst is used, the mercaptan contained in the oil product can be oxidized after the oil product passes through the catalyst bed layer on the premise that the molar concentration of oxygen is greater than that of the mercaptan. During the catalytic reaction, no activating agent and no organic or inorganic alkali are needed, so that the true alkali-free deodorization, alkali residue-free and secondary pollution-free are realized. (3) The reaction speed is high in the catalytic reaction, even if the liquid space velocity is 25h-1Can still ensure the mercaptan to be completely removed at high space velocityAnd (4) oxidizing. (4) When the activity of the catalyst is reduced or the catalyst is invalid, the surface of the catalyst can be washed by water, and the activity is recovered after the catalyst is dried, so that the catalyst is convenient to regenerate and long in service life. (5) When the catalyst is used for converting mercaptan contained in light oil products such as naphtha, gasoline, aviation kerosene, lamp oil, diesel oil and the like, if the molar concentration of dissolved oxygen in the light oil products is greater than that of the mercaptan, air does not need to be introduced during the catalytic reaction; of course, in order to ensure the safety, a small amount of air or oxygen can be introduced. Especially when the catalyst of the invention is used for converting mercaptan contained in liquefied petroleum gas, the mercaptan in the liquefied petroleum gas can be oxidized into disulfide only by 'dissolved oxygen' in the liquefied petroleum gas under the catalytic action. The process for converting mercaptan in liquefied petroleum gas by alkali deodorization is fundamentally changed, the process is greatly simplified, the mercaptan is completely converted, and the problem which is solved for a long time and is not solved by people is solved. (6) The spinel type oxide can be used for preparing butadiene by butadiene oxidative dehydrogenation. However, the invention is a new application of the sweetening agent for oil products.
The composition, preparation and conversion of the catalyst of the present invention will be further described with reference to the following examples. The inventive content is not at all restricted thereto.
Examples 1,
Weighing 1.9 kg of talcum, 1.95 kg of kaolin, 1.15 kg of Al (OH)3Putting the mixture into a kneader, uniformly mixing, adding 0.1 kg of polyvinyl alcohol and a proper amount of water, forming into a mud shape, preparing into small balls with the diameter of 3-5 mm by using a ball forming mill, drying, roasting at the temperature of 1000-1600 ℃ in a high-temperature furnace for 16 hours to generate a spherical carrier, identifying the carrier by an X-ray diffraction phase, wherein the main phase is cordierite, the main phase accounts for 96 percent of the weight of the carrier, and the rest of the carrier is magnesium oxide, silicon oxide, aluminum oxide and a composite compound of the oxides.
28 g of Zn (NO) are weighed out3)2·6H2O, 6.8 g Co (NO)3)2·6H2O, 66.6 g Fe (NO)3)3·9H2O and 47.0 g Cr (NO)3)3·9H2Dissolving O in water to prepare 200 ml of solution, adding 56.0 g of citric acid, stirring, dissolving and uniformly mixing.
And (3) adding 140 g of the carrier into the solution, soaking for 0.5 hour, drying at 80-100 ℃, and roasting at 300-500 ℃ for 2 hours to prepare a catalyst, namely a catalyst A, wherein the loading amount of the active component is 10.80% (based on the carrier amount). The chemical formula of the active component is (Zn) by element analysis0.8Co0.2)(Fe0.5Cr0.5)2O4。
The obtained catalyst A is crushed to 20-40 meshes, 10 g of the catalyst A is taken and placed in a glass chromatographic column with the diameter of 15mm, and the height-diameter ratio is about 5. Taking catalytic gasoline containing about 150ppm of mixed mercaptan and subjected to alkaline washing and electric refining to pass through a fixed bed layer of a catalyst A, wherein the liquid space velocity (LHSV) is 25h-1. The catalytic gasoline after passing through the catalyst bed layer does not contain sulfur any moreAlcohol, doctor tests pass, and the copper sheet is qualifiedin corrosion.
Examples 2,
Weighing 1 kg of gamma-alumina balls with the diameter of 3-5 mm produced by a commercially available Shandong aluminum factory, and roasting at 1200-1600 ℃ for 14 hours to prepare the alumina ball-type carrier, wherein the carrier is identified by an X-ray diffraction phase, the main phase is α -alumina, the main phase accounts for 98% of the weight of the carrier, and the rest of the carrier is alumina.
12.0 g of Zn (NO) are weighed out3)2·6H2O, 10.4 g Mg (NO)3)2·6H2O, 46.0 g Fe (NO)3)3·9H2O and 32.4 g Cr (NO)3)3·9H2Dissolving O in water to prepare 120 ml of solution, adding 30 g of citric acid, and uniformly stirring. 60 g of the carrier is taken out after being soaked for 0.5 hour, dried at the temperature of 80-100 ℃ and roasted at the temperature of 300-500 ℃ for 2 hours to prepare the catalyst, namely the catalyst B, and the loading capacity of the active component is about 9.5 percent (based on the carrier quantity). The chemical formula of the active component is (Zn) by element analysis0.6Mg0.4)(Fe0.6Cr0.4)2O4。
Crushing the catalyst B to 20-40 meshes, and placing 10 g of the catalyst B in a glass chromatographic column with the diameter of 15mm, wherein the height-diameter ratio is about 5. Aviation kerosene containing about 80ppm of mixed mercaptans was passed through a fixed bed of catalyst B at a liquid space velocity (LHSV) of 20-1. No mercaptan sulfur exists in the aviation kerosene passing through the catalyst bed layer, and the copper sheet is qualified in corrosion after passing a doctor test.
Examples 3,
Weighing 1.10 kg of light magnesium oxide, 1.70kg of Al (OH)3And 0.2 kg of polyvinyl alcohol, adding a proper amount of water, kneading, preparing pellets with the diameter of 3-5 mm, drying at 80-120 ℃, and roasting at 1200-1600 ℃ for 10-14 hours to obtain the carrier. The carrier is analyzed by polycrystalline X-ray diffraction, the main phase is magnesia-alumina spinel, the weight percentage of the main phase in the carrier is 96.5%, and the rest part of the carrier is magnesia, silicon oxide and a composite compound of the magnesia and the silicon oxide.
14.0 g of Zn (NO) are weighed out3)2·6H2O, 3.4 g Ni (NO)3)2·6H2O, 33.3 g Fe (NO)3)3·9H2O and 23.5 g Cr (NO)3)3·9H2Dissolving O in water to prepare 100 ml of solution, adding 28 g of citric acid, and uniformly stirring. Taking 70 g of the carrier, soaking for 0.5 hour, taking out, drying at 80-100 ℃, and roasting at 300-500 ℃ for 2 hours to prepare the catalyst, namely the catalyst C, wherein the loading amount of the active component is 10.1% (based on the carrier amount). The chemical formula of the active component is (Zn) by element analysis0.5Ni0.5)(Fe0.7Cr0.3)2O4。
Crushing the obtained catalyst C to 20-40 meshes, taking 10 g, and placing the 10 g into a stainless steel adsorption column with pressure and the diameter of 15mm, wherein the height-diameter ratio of a catalyst bed layer is about 5. Taking liquefied petroleum gas containing mixed mercaptan about 100ppm, passing through a fixed bed layer of a catalyst C, wherein the liquid space velocity (LHSV) is 5h-1. The liquefied petroleum gas after passing through the catalyst bed layer does not contain mercaptan any more, and the copper sheet is qualified after corrosion.
Examples 4,
Weighing 0.92 kg of 70%Al2O3Of aluminum paste with 0.39 kg of a mixture containing 92% by weight of SiO2The silica gel is fully and evenly mixed, then 0.02 kg of polyvinyl alcohol and a proper amount of water are added into the mixture to form a paste, a ball forming machine is used for preparing small balls with the diameter of 3-5 mm,drying, roasting at the high temperature of 1000-1600 ℃ for 16 hours to generate a spherical carrier, and identifying the carrier by an X-ray diffraction phase, wherein the main phase is mullite, the main phase accounts for 97% of the weight of the carrier, and the rest of the carrier is silicon oxide, aluminum oxide and a composite compound of the silicon oxide and the aluminum oxide.
8.0 g of Zn (NO) are weighed out3)2·6H2O, 2.0 g Co (NO)3)2·6H2O and 32.5 g Fe (NO)3)3·9H2Dissolving O in water to prepare 60 ml of solution, adding 16.0 g of citric acid, and uniformly stirring. And (3) taking 30 g of the carrier, soaking for 0.5 hour, taking out, drying, and roasting at 300-500 ℃ for 2 hours to prepare a catalyst, namely a catalyst D, wherein the loading amount of the active component is 9.8% (based on the carrier amount). The chemical formula of the active component is (Zn) by element analysis0.7Co0.3)Fe2O4。
The obtained catalyst D is crushed to 20-40 meshes, 10 g of the catalyst D is placed in a glass chromatographic column with the diameter of 15mm, and the height-diameter ratio is about 5. Taking diesel oil containing about 80ppm of mercaptan, and passing the diesel oil through a fixed bed of a catalyst D, wherein the liquid space velocity (LHSV) is 10h-1. The diesel oil after passing through the catalyst bed layer does not contain mercaptan any more, and the doctor test passes, so that the copper sheet corrosion is qualified.
Examples 5,
6.0 g of Zn (NO) are weighed out3)2·6H2O, 7.16 g Mn (NO)3)2(50% aqueous solution), 23.0 g Fe (NO)3)2·9H2O and 16.2 g Cr (NO)3)3·9H2Dissolving O in water to prepare 60 ml of solution, adding 14.5 g of citric acid, and uniformly stirring. 30 g of the carrier obtained in the example 1 is taken, dipped for 0.5 hour, taken out and dried, and activated for 2 hours at the temperature of 300-500 ℃ to prepare a catalyst, namely a catalyst E, wherein the loading amount of an active component is 9.5 percent(based on the amount of carrier). The chemical formula of the active component is (Zn) by element analysis0.5Mn0.5)(Fe0.8Cr0.2)2O4。
The obtained catalyst E is crushed to 20-40 meshes, 10 g of the crushed catalyst E is placed in a glass chromatographic column with the diameter of 15mm, and the height-diameter ratio is about 5. Naphtha containing about 80ppm of mercaptans was passed over a fixed bed of catalyst E at a liquid space velocity (LHSV) of 10h-1. The naphtha after passing through the catalyst bed layer does not contain mercaptan any more, and the doctor test passes, so that the copper sheet corrosion is qualified.
Examples 6,
6.0 g of Zn (NO) are weighed out3)2·6H2O, 4.84 g Cu (NO)3)2·3H2O, 23.0 g Fe (NO)3)3·9H2O and 16.2 g Cr (NO)3)3·9H2Dissolving O in water to prepare 60 ml of solution, adding 14.5 g of citric acid, and uniformly stirring. 30 g of the carrier obtained in the example 1 is taken, added with the solution, dipped for 0.5 hour, taken out and dried, and activated for 2 hours at 300-500 ℃ to prepare the catalyst, namely the catalyst F, wherein the loading amount of the active component is 9.9 percent (based on the carrier amount). The chemical formula of the active component is (Zn) by element analysis0.5Cu0.5)(Fe0.8Cr0.2)2O4。
The obtained catalyst F is crushed to 20-40 meshes, 10 g of the catalyst F is taken and placed in a glass chromatographic column with the diameter of 15mm, and the height-diameter ratio is about 5. Taking catalytic gasoline containing about 150ppm of mixed mercaptan and subjected to alkaline washing and electric refining to pass through a fixed bed layer of a catalyst F, wherein the liquid space velocity (LHSV) is 20h-1. The catalytic gasoline after passing through the catalyst bed layer does not contain mercaptan any more, and the doctor test passes, so that the copper sheet corrosion is qualified.
Example 7,
6.0 g of Zn (NO) are weighed out3)2·6H2O, 6.2 g Co (NO)3)24H2O, 23.0 g Fe (NO)3)3·9H2O and 16.2 g Cr (NO)3)3·9H2O dissolved in waterThen, 60 ml of solution is prepared, and 14.5 g of citric acid is added and stirred uniformly. 30G of the carrier obtained in the example 3 is taken, added with the solution, dipped for 0.5 hour, taken out and dried, and activated for 2 hours at 300-500 ℃ to prepare the catalyst, namely the catalyst G, wherein the loading amount of the active component is 10.1 percent (based on the carrier amount). The chemical formula of the active component is (Zn) by element analysis0.5Cd0.5)(Fe0.8Cr0.2)2O4。
The obtained catalyst G is crushed to 20-40 meshes, 10G of the catalystG is placed in a glass chromatographic column with the diameter of 15mm, and the height-diameter ratio is about 5. Taking aviation kerosene containing about 80ppm of mercaptan, and passing the aviation kerosene through a fixed bed of a catalyst G, wherein the liquid space velocity (LHSV) is 20h-1. The aviation kerosene which passes through the catalyst bed layer does not contain mercaptan any more, and the doctor test passes, so that the copper sheet is qualified in corrosion.
The carrier prepared by the method of the embodiment of the invention is passivated by high-temperature treatment, and the carrier and the active component do not have chemical reaction at the temperature of preparing the catalyst, so that the function of the active component is effectively exerted.
Claims (8)
1. A catalyst for converting mercaptans contained in hydrocarbon oil, characterized in that: the active component of the catalyst is spinel type oxide.
2. The catalyst of claim 1, wherein: the general formula of the spinel type oxide is:
(AXA’1-X)(BYB’1-Y)2O4wherein A, A 'is respectively a metal element selected from Zn, Co, Ni, Mg, Mn, Cu and Cd, B is a metal element Fe, B' is a metal element selected from Cr, Co, Ni and Mn, X is more than or equal to 0 and less than or equal to 1, Y is more than or equal to 0.4 and less than or equal to 1.0, and the active component is directly loaded on mullite, cordierite, magnesia-alumina spinel or α -Al2O3On a carrier as the main phase.
3. The catalyst of claim 2, wherein: A. a' is respectively a metal element selected from Zn, Co andMn; b' is metal element Cr.
4. A catalyst according to claim 2 or 3, characterized in that: the spinel type oxide has the chemical formula of (Zn)0.8Co0.2)(Fe0.5Cr0.5)2O4、(Zn0.6Mg0.4)(Fe0.6Cr0.4)2O4、(Zn0.5Ni0.5)(Fe0.7Cr0.3)2O4、(Zn0.7Co0.3)Fe2O4、(Zn0.5Mn0.5)(Fe0.8Cr0.2)2O4、(Zn0.5Cu0.5)(Fe0.8Cr0.2)2O4Or (Zn)0.5Cd0.5)(Fe0.8Cr0.2)2O4。
5. The catalyst according to one of claims 2 to 4, characterized in that: the carrier of the catalyst is a carrier taking cordierite or magnesia-alumina spinel as a main phase, and the weight percentage of the main phase in the carrier is more than or equal to 80 percent.
6. The catalyst according to one of claims 2 to 4, characterized in that: the loading amount of the active component on the carrier is 5-15% (weight).
7. The catalyst with spinel type oxide as active component is used in converting mercaptan in hydrocarbon oil.
8. The catalyst with spinel type oxide as active component is used in converting mercaptan in liquefied petroleum gas, naphtha, gasoline, aviation kerosene, lamp oil or diesel oil.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 00107681 CN1206031C (en) | 2000-05-23 | 2000-05-23 | Catalyst for converting mercaptan contained in hydrocarbon oil |
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| CN 00107681 CN1206031C (en) | 2000-05-23 | 2000-05-23 | Catalyst for converting mercaptan contained in hydrocarbon oil |
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| CN 00107681 Expired - Lifetime CN1206031C (en) | 2000-05-23 | 2000-05-23 | Catalyst for converting mercaptan contained in hydrocarbon oil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105195134A (en) * | 2015-08-27 | 2015-12-30 | 四川正洁科技有限责任公司 | Catalyst for deodorizing mineral oil and preparation method and use method of catalyst |
| CN109999818A (en) * | 2019-04-22 | 2019-07-12 | 广州大学 | A kind of activation persulfate Magnetic solid phases catalyst and the preparation method and application thereof |
-
2000
- 2000-05-23 CN CN 00107681 patent/CN1206031C/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105195134A (en) * | 2015-08-27 | 2015-12-30 | 四川正洁科技有限责任公司 | Catalyst for deodorizing mineral oil and preparation method and use method of catalyst |
| CN105195134B (en) * | 2015-08-27 | 2017-11-17 | 杨光 | Mineral oil deodorizing catalyst and its preparation and application |
| CN109999818A (en) * | 2019-04-22 | 2019-07-12 | 广州大学 | A kind of activation persulfate Magnetic solid phases catalyst and the preparation method and application thereof |
| CN109999818B (en) * | 2019-04-22 | 2021-07-13 | 广州大学 | Activated persulfate magnetic solid-phase catalyst and preparation method and application thereof |
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