CN110064405B - Preparation method of hydrotreating catalyst with desulfurization activity - Google Patents
Preparation method of hydrotreating catalyst with desulfurization activity Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/187—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with manganese, technetium or rhenium
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- C—CHEMISTRY; METALLURGY
- 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
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
- C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
- C10G45/06—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof
- C10G45/08—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof in combination with chromium, molybdenum, or tungsten metals, or compounds thereof
Abstract
A method for preparing a hydrotreating catalyst having desulfurization activity, comprising the steps of: step 1, preparing a macroporous carrier of phosphorus-containing alumina or phosphorus-modified alumina material; step 2, impregnating the porous carrier with a metal I solution, curing, drying and roasting to obtain a catalyst precursor, wherein the metal I solution is a NiMo solution containing Ni and Mo elements; step 3, dipping the catalyst precursor into a II-type metal solution containing an organic auxiliary agent, and then curing and drying the catalyst precursor without roasting to obtain a final catalyst; the II-type metal solution is a CoMo solution containing Co and Mo elements, and the I-type metal solution and the II-type metal solution are not a NiMo solution or a CoMo solution at the same time. The method adopts metal solution to dip step by step, provides active site combinations with different types and combinations of different types of metals, and generates higher hydrodesulfurization activity than the traditional simple I type catalyst and simple II type catalyst.
Description
Technical Field
The invention relates to a preparation method of a high-activity hydrogenation catalyst, in particular to a NiCoMo high-activity hydrogenation desulfurization catalyst, and a preparation method and application thereof.
Background
The existence of impurities such as sulfur, nitrogen, metal and the like in the distillate oil can not only influence the oxidation stability of the finished oil, but also discharge SO2、NO2And the like. The removal of impurities from the distillate by hydrotreating is a very necessary measure. Fraction oil hydrotreating targetNamely, organic sulfur in the raw materials is converted into hydrogen sulfide, and organic nitrogen is converted into ammonia gas. The fraction oil hydrogenation treatment is a process of contacting fraction oil and hydrogen with a catalyst under a certain temperature and pressure condition to remove impurities and saturate aromatic hydrocarbon. Therefore, it is important to prepare a catalyst that develops a preparation method of a hydrotreating catalyst to obtain a high activity.
At present, the methods for desulfurization, denitrification and dearomatization of diesel oil fractions generally adopt a two-stage method, namely, a first stage of hydrodesulfurization and denitrification, and a second stage of hydrogenation dearomatization. Conventional hydrodesulfurization and denitrogenation catalysts generally comprise a carrier and a group VIB and/or group VIII active metal component loaded on the carrier, wherein the most common group VIB metals are molybdenum and tungsten, and the group VIII metals are nickel and cobalt, and the catalysts also often contain auxiliary agents such as phosphorus, boron and the like. The catalyst is generally prepared by supporting the active component on a support, for example by impregnation, and then converting it to the oxidized state by drying and calcination at high temperature. The catalyst is presulfided to convert it to the sulfided state prior to use in hydroprocessing. Therefore, a large amount of energy is wasted, the cost of the catalyst is increased, and the catalyst performance is reduced because some non-ideal phases with low or even no activity are formed by high-temperature roasting after the active metal is loaded.
It is reported that the organic compound is added into the metal impregnation liquid and impregnated on the porous carrier, so that more high-activity II-type active phase can be generated, and simultaneously, the activity loss caused by metal aggregation in the high-temperature vulcanization process of the catalyst can be prevented, thereby improving the activity of the hydrotreating catalyst.
A number of patents disclose the use of various organic compounds, such as oxygen-containing organic compound polyols or etherified (WO96/41848, US3954673, US 4012340).
Patent JP 04166231 discloses a method for preparing a hydrotreating catalyst by impregnating a porous support with a metal solution, drying the impregnated support at a temperature of not higher than 200 ℃, and subjecting the dried support to a drying step after contacting the support with a polyol.
EP 0601722 discloses a method for preparing a catalyst, characterized in that a porous alumina carrier is impregnated with an aqueous metal solution containing a glycol, and the impregnated carrier is subjected to a primary drying step without being subjected to a calcination process to prepare a finished catalyst.
US 6218333 discloses a method of preparing a hydroprocessing catalyst by combining a porous support with an active metal component to form a catalyst precursor having volatiles. The catalyst precursor is treated with a sulfur-containing compound, and volatiles are released from the catalyst precursor under dry conditions. However, these improvements are not sufficient to meet the increasingly stringent fuel requirements of refineries.
The high activity of the hydrotreating catalyst can make the hydrotreating process conditions moderate, such as low reaction temperature, or obtain products with better quality under the same conditions. Therefore, how to develop a highly active hydrotreating catalyst is an object of constant search by those skilled in the art.
Disclosure of Invention
The invention aims to provide a preparation method of a hydrotreating catalyst with desulfurization activity.
In order to achieve the above object, the present invention provides a method for preparing a hydrotreating catalyst having desulfurization activity, comprising the steps of:
step 1, preparing a macroporous carrier of phosphorus-containing alumina or phosphorus-modified alumina material;
step 2, impregnating the porous carrier with a metal I solution, curing, drying and roasting to obtain a catalyst precursor, wherein the metal I solution is a NiMo solution containing Ni and Mo elements;
step 3, dipping the catalyst precursor into a II-type metal solution containing an organic auxiliary agent, and then curing and drying the catalyst precursor without roasting to obtain a final catalyst; the II-type metal solution is a CoMo solution containing Co and Mo elements, and the I-type metal solution and the II-type metal solution are not a NiMo solution or a CoMo solution at the same time.
And 2, obtaining metal particles with larger sizes through a roasting process.
In the preparation method of the hydrotreating catalyst with desulfurization activity, the organic auxiliary agent in the step 2 contains alcohols and/or organic acids.
The preparation method of the hydrotreating catalyst with desulfurization activity of the invention comprises the following steps of the organic auxiliary agent in step 3: the organic auxiliary agent is contained in an amount of 0.01 to 3 mol per mol of the active metal based on the metal II solution.
In the preparation method of the hydrotreating catalyst with desulfurization activity of the present invention, the drying in step 3 is a drying method commonly used in the art, such as vacuum drying or atmospheric drying, and is not particularly limited, and may be one-time or multi-step drying. .
According to the preparation method of the hydrotreating catalyst with desulfurization activity, the drying temperature in the step 3 is lower than 260 ℃.
According to the preparation method of the hydrotreating catalyst with desulfurization activity, the drying temperature in the step 3 is 100-260 DEG C
According to the preparation method of the hydrotreating catalyst with desulfurization activity, the alcohol organic auxiliary agent is polyethylene glycol.
According to the preparation method of the hydrotreating catalyst with desulfurization activity, the organic acid organic auxiliary agent is citric acid.
According to the preparation method of the hydrotreating catalyst with desulfurization activity, the ratio of the I-type active site to the II-type active site in the catalyst is within 0.2-0.6.
The preparation method of the hydrotreating catalyst with desulfurization activity comprises the step 2, wherein the drying temperature is 100-300 ℃, and the roasting temperature is 400-550 ℃.
The invention has the beneficial effects that:
a hydrotreating catalyst having a combination of different types of metals and different types of active sites and having a high desulfurization activity is provided.
Drawings
FIG. 1 is a flow chart of a process for producing a catalyst in example 1 of the present invention;
FIG. 2 is a flow chart of the production process of the catalyst in example 2 of the present invention.
Detailed Description
The technical solutions of the present invention are described in detail below with reference to specific examples so as to facilitate understanding of the objects and technical contents of the present invention, and the embodiments are only for illustration and are not intended to limit the present invention.
A method for preparing a hydrotreating catalyst having desulfurization activity, comprising the steps of:
step 1, preparing a macroporous carrier of phosphorus-containing alumina or phosphorus-modified alumina material;
step 2, impregnating the porous carrier with a metal I solution, curing, drying and roasting to obtain a catalyst precursor, wherein the metal I solution is a NiMo solution containing Ni and Mo elements;
step 3, dipping the catalyst precursor into a II-type metal solution containing an organic auxiliary agent, and then curing and drying the catalyst precursor without roasting to obtain a final catalyst; the II-type metal solution is a CoMo solution containing Co and Mo elements, and the I-type metal solution and the II-type metal solution are not a NiMo solution or a CoMo solution at the same time.
In the preparation method of the hydrotreating catalyst with desulfurization activity, the organic auxiliary agent in the step 2 contains alcohols and/or organic acids.
The preparation method of the hydrotreating catalyst with desulfurization activity of the invention comprises the following steps of the organic auxiliary agent in step 3: the organic auxiliary agent is contained in an amount of 0.01 to 3 mol per mol of the active metal based on the metal II solution.
In the preparation method of the hydrotreating catalyst with desulfurization activity of the present invention, the drying in step 3 is a drying method commonly used in the art, such as vacuum drying or atmospheric drying, and is not particularly limited, and may be one-time or multi-step drying. .
According to the preparation method of the hydrotreating catalyst with desulfurization activity, the drying temperature in the step 3 is lower than 260 ℃.
According to the preparation method of the hydrotreating catalyst with desulfurization activity, the drying temperature in the step 3 is 100-260 DEG C
According to the preparation method of the hydrotreating catalyst with desulfurization activity, the alcohol organic auxiliary agent is polyethylene glycol.
According to the preparation method of the hydrotreating catalyst with desulfurization activity, the organic acid organic auxiliary agent is citric acid.
According to the preparation method of the hydrotreating catalyst with desulfurization activity, the ratio of the I-type active site to the II-type active site in the catalyst is within 0.2-0.6.
The preparation method of the hydrotreating catalyst with desulfurization activity comprises the step 2, wherein the drying temperature is 100-300 ℃, and the roasting temperature is 400-550 ℃.
Example 1 preparation of Ni/CoMo catalyst type I/II C3 (according to the invention)
Step 1, extruding, drying and roasting pseudo-boehmite to prepare clover-shaped A12O3And (3) a carrier. Taking 70g of prepared A12O3The carrier is soaked by 5.0g of phosphoric acid with the concentration of 85 percent, and after being cured for 4 hours, the carrier is dried for 3 hours at the temperature of 120 ℃ to obtain the phosphoric acid modified alumina carrier.
Step 2, NiMo solution was prepared by dissolving ammonium heptamolybdate (15g) and nickel nitrate hexahydrate (11.6g) in 50ml of an aqueous ammonia (6%) solution. NiMo solution is added into the phosphorus modified carrier, and after soaking, the extrudate is cured at room temperature for 6 hr, dried at 120 deg.c overnight and roasted at 400 deg.c for 4 hr to prepare the catalyst precursor.
And 3, dissolving ammonium heptamolybdate (15g) and cobalt nitrate hexahydrate (18.8g) in an aqueous solution of citric acid to prepare a uniform and transparent CoMo solution. After the catalyst precursor was impregnated with a CoMo-CA (citric acid, citric acid CA/Mo ═ 0.1, molar ratio) mixed solution, it was aged at room temperature for 6 hours and dried at 100 ℃ for 6 hours to obtain Ni/CoMo type I/II catalyst C1.
EXAMPLE 2 preparation of Co/NiMo catalyst type I/II C2 (according to the invention)
Step 1, extruding, drying and roasting pseudo-boehmite to prepare clover-shaped A12O3And (3) a carrier. Taking 70g of prepared A12O3The carrier is soaked by 5.0g of phosphoric acid with the concentration of 85 percent, and after being cured for 4 hours, the carrier is dried for 3 hours at the temperature of 120 ℃ to obtain the phosphoric acid modified alumina carrier.
Step 2, a CoMo solution was prepared by dissolving ammonium heptamolybdate (15g) and cobalt nitrate hexahydrate (18.8g) in 50ml of an aqueous ammonia (6%) solution. The CoMo solution was added to the above phosphorus-modified support, and after impregnation, the extrudate was aged at room temperature for 6 hours, dried at 100 ℃ overnight, and calcined at 550 ℃ for 4 hours to prepare a catalyst precursor.
And 3, dissolving ammonium heptamolybdate (15g) and nickel nitrate hexahydrate (11.6g) in an aqueous solution of citric acid to prepare a uniform and transparent NiMo solution. After impregnating the catalyst precursor with a NiMo-CA (citric acid, citric acid CA/Mo ═ 0.1, molar ratio) mixed solution, the catalyst precursor was aged at room temperature for 6 hours and dried at 260 ℃ for 6 hours, to obtain a type I/II Co/NiMo catalyst C2.
Example 3 preparation of Ni/CoMo catalyst type I/II C3 (according to the invention)
Step 1, extruding, drying and roasting pseudo-boehmite to prepare clover-shaped A12O3And (3) a carrier. Taking 70g of prepared A12O3The carrier is soaked by 5.0g of phosphoric acid with the concentration of 85 percent, and after being cured for 4 hours, the carrier is dried for 3 hours at the temperature of 120 ℃ to obtain the phosphoric acid modified alumina carrier.
Step 2, NiMo solution was prepared by dissolving ammonium heptamolybdate (15g) and nickel nitrate hexahydrate (11.6g) in 50ml of an aqueous ammonia (6%) solution. NiMo solution is added into the phosphorus modified carrier, and after soaking, the extrudate is cured at room temperature for 6 hr, dried at 250 deg.c overnight, and roasted at 450 deg.c for 4 hr to prepare the catalyst precursor.
Step 3, ammonium molybdate (15g) and cobalt nitrate hexahydrate (18.8g) were dissolved in an aqueous solution of citric acid and polyethylene glycol (CA/Mo ═ 0.05, PEG/Mo ═ 0.05), to prepare a uniform and transparent CoMo solution. The catalyst precursor was impregnated with a mixed solution of CoMo-CA-PEG, followed by aging at room temperature for 6 hours and drying at 190 ℃ for 6 hours to obtain Ni/CoMo type I/II catalyst C3.
Comparative example 1 preparation of type I NiCoMo catalyst DC1 (not according to the invention)
Step 1, extruding, drying and roasting pseudo-boehmite to prepare a product IIILeaf-shaped A12O3And (3) a carrier. Taking 70g of prepared A12O3The carrier is soaked by 5.0g of phosphoric acid with the concentration of 85 percent, and after being cured for 4 hours, the carrier is dried for 3 hours at the temperature of 120 ℃ to obtain the phosphoric acid modified alumina carrier.
Step 2, NiMo solution was prepared by dissolving ammonium heptamolybdate (15g) and nickel nitrate hexahydrate (11.6g) in 50ml of an aqueous ammonia (6%) solution. The NiMo solution was added to the above phosphorus-modified support, and after impregnation, the extrudate was aged at room temperature for 6 hours and dried at 120 ℃ to obtain a catalyst precursor. (non-calcined)
And 3, dissolving ammonium molybdate (15g) and cobalt nitrate hexahydrate (18.8g) in an aqueous solution of citric acid to prepare a uniform and transparent CoMo solution. And (3) soaking the catalyst precursor in a CoMo solution containing citric acid, curing at room temperature for 6 hours, drying at 120 ℃ overnight, and roasting at 400-550 ℃ for 4 hours to obtain a roasted catalyst DC 1. (with roasting)
Comparative example 2 preparation of type II NiCoMo catalyst DC2 (not according to the invention)
Step 1, extruding, drying and roasting pseudo-boehmite to prepare clover-shaped A12O3And (3) a carrier. Taking 70g of prepared A12O3The carrier is soaked by 5.0g of phosphoric acid with the concentration of 85 percent, and after being cured for 4 hours, the carrier is dried for 3 hours at the temperature of 120 ℃ to obtain the phosphoric acid modified alumina carrier.
Step 2, NiMo solution was prepared by dissolving ammonium heptamolybdate (15g) and nickel nitrate hexahydrate (11.6g) in 50ml of an aqueous ammonia (6%) solution. NiMo solution is added into the phosphorus modified carrier, and after soaking, the extrudate is cured at room temperature for 6 hr and dried at 120 deg.c to obtain the catalyst precursor. (non-calcined)
And 3, dissolving ammonium heptamolybdate (15g) and cobalt nitrate hexahydrate (18.8g) in an aqueous solution of citric acid to prepare a uniform and transparent CoMo solution. And (3) soaking the catalyst precursor in a CoMo mixed solution containing citric acid, curing at room temperature for 6 hours, and drying at 100-260 ℃ for 6 hours to obtain a II-type catalyst DC 2. (non-calcined)
The evaluation of the catalyst used was carried out by sulfurizing aviation kerosene fractions containing carbon disulfide at 260 ℃ and 370 ℃ for 8 hours, respectively, feeding the feed oil and then stabilizing the feed oil under the reaction conditions for 8 hours, and then starting the hydrodesulfurization reaction test. When the catalyst is evaluated, the reaction temperature is adjusted to ensure that the desulfurization rate is 96 w%, and the denitrification rate can be achieved by the low reaction temperature of the catalyst, which shows that the catalyst has higher hydrodesulfurization activity. It can be seen that catalyst C3 of example 3 has the highest hydrodesulfurization activity.
TABLE 1 Properties of the raw oils
| Raw oil | VGO |
| Density, g/ml | 0.9 |
| Sulfur, w% | 0.51 |
| Nitrogen, w% | 0.15 |
| Carbon residue, w% | 0.05 |
| Distillation range, deg.C | |
| IBP/10％ | 290/345 |
| 30％/50％ | 360/390 |
| 70％/90％ | 400/435 |
| 95％/EBP | 445/460 |
TABLE 2 hydrodesulfurization reaction Process conditions
| Reaction pressure, MPa | 7 |
| LHSV,h-1 | 1.0 |
| H2Oil ratio, V/V | 1000 |
TABLE 3 comparison of hydrodenitrogenation activity of catalysts
The present invention is capable of other embodiments, and various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (6)
1. A method for preparing a hydrotreating catalyst having desulfurization activity, characterized by comprising the steps of:
step 1, preparing a macroporous carrier of phosphorus-containing alumina or phosphorus-modified alumina material;
step 2, impregnating the porous carrier with a metal I solution, curing, drying and roasting to obtain a catalyst precursor, wherein the metal I solution is a NiMo solution containing Ni and Mo elements;
step 3, dipping the catalyst precursor into a II-type metal solution containing an organic auxiliary agent, and then curing and drying the catalyst precursor without roasting to obtain a final catalyst; the II-type metal solution is a CoMo solution containing Co and Mo elements;
the organic auxiliary agent is citric acid and polyethylene glycol.
2. The method for preparing a hydroprocessing catalyst with desulfurization activity according to claim 1, wherein the amount of the organic auxiliary agent used in step 3 is: the organic auxiliary agent is contained in an amount of 0.01 to 3 mol per mol of the active metal based on the metal II solution.
3. The method for preparing a hydroprocessing catalyst having desulfurization activity according to claim 1, wherein the drying in the step 3 is one or more times in steps.
4. The method for preparing a hydrotreating catalyst having desulfurization activity according to claim 1, characterized in that the drying temperature in step 3 is 100 to 260 ℃.
5. The method of claim 1, wherein the ratio of the group I active sites to the group II active sites in the catalyst is in the range of 0.2 to 0.6.
6. The method for preparing a hydrotreating catalyst with desulfurization activity according to claim 1, characterized in that the drying temperature in step 2 is 100 to 300 ℃ and the calcination temperature is 400 to 550 ℃.
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| WO2021218982A1 (en) * | 2020-04-28 | 2021-11-04 | 中国石油化工股份有限公司 | Hydrogenation catalyst and preparation method therefor and use thereof |
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| US4318801A (en) * | 1979-09-04 | 1982-03-09 | Gulf Research & Development Company | Supported nickel-molybdenum catalyst, preparation thereof, and hydrodesulfurization of hydrocarbon fractions using same |
| US6231754B1 (en) * | 1996-02-02 | 2001-05-15 | Exxon Research And Engineering Company | High temperature naphtha desulfurization using a low metal and partially deactivated catalyst |
| CN1055955C (en) * | 1997-11-24 | 2000-08-30 | 中国石油化工总公司 | Hydrogenation catalyst and preparation thereof |
| CN100587038C (en) * | 2006-01-27 | 2010-02-03 | 中国石油化工股份有限公司 | Hydrogenation method for producing good quality catalytic cracking material |
| CN101491766B (en) * | 2008-01-23 | 2011-06-22 | 中国石油化工股份有限公司 | Preparation method of hydrogenation catalyst |
| CN102580757B (en) * | 2011-01-13 | 2016-08-10 | 中国石油化工股份有限公司 | A kind of hydrotreating catalyst and preparation thereof and application |
| CN103374393A (en) * | 2012-04-26 | 2013-10-30 | 中国石油化工股份有限公司 | Hydrotreatment method for hydrocarbon oil |
| EP2918339B1 (en) * | 2012-11-08 | 2019-05-22 | China Petroleum & Chemical Corporation | Hydrogenation catalyst and manufacturing method therefor and use thereof |
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