CN103769220A - Preparation method of catalyst for distillate oil hydro-treatment - Google Patents
Preparation method of catalyst for distillate oil hydro-treatment Download PDFInfo
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Abstract
The invention discloses a preparation method of a catalyst for distillate oil hydro-treatment. The preparation method adopts a step-by-step spraying and soaking technology and comprises the following steps: loading at least one component selected from a VIB group metal, organic alcohol, and organic sugar onto a catalyst carrier, then loading a VIII group metal and an organic acid on the catalyst carrier, and finally drying so as to obtain the catalyst for hydro-treatment. The preparation method has the advantages of little use amount of organic compound, small viscosity of impregnation solution, and easy and practicable preparation; and furthermore the prepared hydro-treatment catalyst has the advantages of high activity and good stability. The hydro-treatment catalyst is especially suitable for being applied to a diesel oil hydro-desulfurization technology.
Description
Technical field
The present invention relates to a kind of preparation method of catalyst for hydrogenation of fraction oil, especially for the preparation method of the hydrotreating catalyst of deep hydrodesulfurizationof of diesel oil.
Background technology
Along with heaviness, in poor quality and the sulfur crude processing amount of crude oil are year by year the trend rising, the impurity contents such as sulphur, nitrogen and colloid in diesel raw material are increased.On the other hand, increasingly strict along with environmental regulation, more and more harsher to the requirement of diesel product quality, especially more strict to the requirement of the sulfur content in diesel oil, Cetane number and polycyclic aromatic hydrocarbon content, secondary processing diesel oil must could meet through deep hydrofinishing the diesel quality index request of high standard.
Along with the low sulfuration of diesel oil, it is more and more important that Hydrofining Technology seems.Although can increase reactor volume, increase recycle hydrogen de H by improving reaction temperature, reduction reaction velocity, reconstruction or new device
2s device, reduce cut cut point and adopt more the modes such as high activated catalyst to improve desulfurization depth, but improving reaction temperature can increase energy consumption and shorten catalyst service life, reduce reaction velocity and can reduce treating capacity, reconstruction or new device can increase plant investment and catalyst amount, by contrast, most economical and easy method is to select optimal high activity deep hydrodesulfurizationof of diesel oil catalyst according to device working condition.
CN1938087B, US7737071B2, EP1733787A1 have introduced a kind of preparation method of hydrogenation catalyst, comprise: with compound and the organic acid solution impregnating carrier of the compound that comprises group vib metal, phosphorus containing components, group VIII metal, then at 200 ℃ or lower temperature, be dried, obtain catalyst.In catalyst, coming from organic acid C content is 2% ~ 14%.
EP0870003B2 has introduced a kind of method of preparing hydrogenation catalyst, comprise: with the compound of the compound that comprises group vib metal, group VIII metal and the solution impregnating carrier of Organic Alcohol and/or sugar, then at 200 ℃ or lower temperature, be dried, obtain catalyst.In catalyst, the C content that comes from Organic Alcohol and/or sugar is 2% ~ 10%.
The defect of above-mentioned patent is that in catalyst, organic compound content is too high, and in preparation process, because dipping solution viscosity causes greatly catalyst to prepare difficulty to be increased, preparation time is long, but also can affect the distribution of active metal on catalyst etc.Due to reasons such as organic compound content are high, and solution viscosity is large, skewness, can make catalyst in high temperature vulcanized process, produce excessive sulfurate activity and pile up neatly mutually layer, affect the decentralization of active metal, and then affect the activity of catalyst.In addition, adopt separately organic acid, or adopt Organic Alcohol separately or/and sugared in above-mentioned patented method, though can improve to a certain extent like this activity of catalyst, the activity of catalyst need further raising.
Summary of the invention
For the deficiencies in the prior art part, the invention provides the preparation method of the catalyst for hydrogenation of fraction oil that a kind of activity is high.The prepared dipping solution viscosity of the method is little, prepares simple.
The preparation method of hydrotreating catalyst of the present invention, described catalyst is take aluminium oxide as carrier, take at least one group vib metal and at least one group VIII metal as hydrogenation active metals, in catalyst, contain organic compound, organic compound come from organic acid and be selected from Organic Alcohol and organic sugar at least one, this catalyst is to adopt infusion process load regulation group vib metal on alumina support, group VIII metal and organic compound, the addition of organic compound accounts for the 1.0wt% ~ 1.8wt% of hydrotreating catalyst weight in C, be preferably 1.2 wt% ~ 1.6 wt %, process comprises:
(1) prepare respectively dipping solution I and dipping solution II, wherein dipping solution I is by formulated containing at least one and water in group vib metal and Organic Alcohol and organic sugar, dipping solution II is by formulated containing group VIII metallic compound and organic acid, water, wherein organic acid addition take C with the mol ratio of group VIII metal as 0.01 ~ 0.70, be selected from least one in Organic Alcohol and organic sugar take C with the mol ratio of group vib metal as 0.01 ~ 0.40;
(2) first use dipping solution I oxide impregnation alumina supporter, after dry at the temperature below 200 ℃, then with dipping solution II dipping, dry at the temperature below 200 ℃, obtain hydrotreating catalyst.
Described hydrotreating catalyst, take at least one group vib metal and at least one group VIII metal as hydrogenation active metals, take the weight of catalyst as benchmark, hydrogenation active metals, take the weight content of oxide as 14% ~ 50%, is preferably 15% ~ 40%.In described hydrotreating catalyst, group vib metal is preferably Mo and/or W, and group VIII metal is preferably Ni and/or Co.In described hydrotreating catalyst, group VIII metal/(group vib metal+group VIII metal) is take the weight ratio of the weight ratio (being abbreviated as VIII/(VIB+VIII in the present invention) of oxide) as 0.30 ~ 0.55.
It is at least one in 2 ~ 10 binary acid that described organic acid is selected from carbon number, is preferably one or more in citric acid, citric anhydride, isocitric acid, malic acid, tartaric acid, oxalic acid, butanedioic acid, glutaric acid, adipic acid, benzoic acid, phthalandione, isophathalic acid, salicylic acid, malonic acid; It is one or more in 3 ~ 10 fatty alcohol and dihydroxylic alcohols that described Organic Alcohol is selected from carbon number, is preferably one or more in fatty alcohol, ethylene glycol, propyleneglycoles, glycerine, three methylol ethane, three methylol propane, divinyl ethylene glycol, two propyleneglycoles, trimethylene ethylene glycol, trietbhlene glycol, tributylene glycol, tetrem allyl diglycol, tetrapropylene ethylene glycol, polyethylene glycol, divinyl Propylene Glycol, divinyl ethohexadiol, divinyl propyl glycol, divinyl butyl glycol; It is at least one in 3 ~ 10 monose, disaccharides and polysaccharide that described organic sugar is selected from carbon number.
In described catalyst, can also contain auxiliary agent phosphorus, the weight content of phosphorus in catalyst is 0.01% ~ 2.5%.
The character of hydrotreating catalyst of the present invention is as follows: pore volume is 0.3 ~ 1.3ml/g, and specific area is 150 ~ 400m
2/ g.
In the inventive method, while adopting dipping solution I or dipping solution II to flood, preferably adopt the saturated method that sprays, can adopt one or many dipping, after each dipping all will through 200 ℃ or lower temperature dry.In the inventive method, the concentration of maceration extract forms (content) by water absorption rate and desired catalyst and determines.
Described alumina support can adopt conventional method preparation, can contain a small amount of auxiliary agent as one or more in silicon, titanium, magnesium, boron, zirconium in alumina support, and auxiliary agent content is counted 0.1% ~ 10% of carrying alumina body weight with element.The character General Requirements of described alumina support is as follows: pore volume is 0.3 ~ 1.5ml/g, and specific area is 150 ~ 450m
2/ g.
The inventive method adopts substep to spray method, first at least one in group vib metal, Organic Alcohol and organic sugar is loaded in catalyst carrier, and then group VIII metal and organic acid are loaded in catalyst carrier.The method can be in the situation that organic compound consumption be less, first adopt the weak Organic Alcohol (sugar) of complexing to flood with the maceration extract of group vib metal, utilize the polarity of Organic Alcohol (sugar), make group vib metal first be dispersed in carrier surface, further adopt afterwards organic acid and the part group VIII metal that complexing is stronger to form appropriate complex compound, being conducive to group VIII metal is combined with the height of group vib metal and is dispersed on alumina support, form the more easily state of sulfuration, make VIB, VIII family metal obtains quick full cure, be conducive to VIB and form the active phase of more II class with group VIII metal, thereby make catalyst there is higher hydrogenation activity.In addition, in dipping solution, the consumption of organic compound is less, makes maceration extract not have higher viscosity, and this makes preparation become more easily enforcement.
The inventive method, preferably adopt higher VIII/(VIB+VIII) weight ratio, and group vib and Organic Alcohol (sugar), group VIII and organic acid substep spray method to alumina support, in the situation that organic compound consumption is less, make catalyst there is higher hydrogenation activity.
Catalyst for hydrogenation of fraction oil of the present invention is applicable to the cuts such as liquefied gas, gasoline, kerosene, diesel oil, wax oil, is particularly useful in diesel hydrogenation for removal sulphur technique.
The specific embodiment
In the present invention, specific area and pore volume employing low temperature liquid nitrogen determination of adsorption method.In the present invention, wt% represents mass fraction.
Below in conjunction with embodiment, the present invention is further detailed explanation.
Embodiment 1
100 g alumina supports are placed in and roll pot, under rotation condition, spray into 80ml with atomizing type and contain 22.9g molybdenum trioxide to rolling alumina support in pot, the aqueous solution of 0.9g ethylene glycol, after solution has sprayed, be rotated further 30 minutes rolling in pot, then place 18 hours, at 110 ℃ dry 5 hours.Take after weight and be placed in again and roll pot, under rotation condition, in pot, spray into 35ml with atomizing type again and contain 15.3g basic cobaltous carbonate to rolling, 3.8g lemon aqueous acid, after solution has sprayed, be rotated further 30 minutes rolling in pot, then place 18 hours, at 110 ℃, be dried 5 hours, make finished catalyst A.
Embodiment 2
100 g alumina supports are placed in and roll pot, under rotation condition, spray into 80ml with atomizing type and contain 21.5g molybdenum trioxide to rolling alumina support in pot, the aqueous solution of 0.9g ethylene glycol, after solution has sprayed, be rotated further 30 minutes rolling in pot, then place 18 hours, at 110 ℃ dry 5 hours.Take after weight and be placed in again and roll pot, under rotation condition, in pot, spray into 35ml with atomizing type again and contain 17.4g basic cobaltous carbonate to rolling, 3.5g lemon aqueous acid, after solution has sprayed, be rotated further 30 minutes rolling in pot, then place 18 hours, at 110 ℃, be dried 5 hours, make finished catalyst B.
Embodiment 3
100 g alumina supports are placed in and roll pot, under rotation condition, spray into 80ml with atomizing type and contain 22.9g molybdenum trioxide to rolling alumina support in pot, the aqueous solution of 2.0g glycerine, after solution has sprayed, be rotated further 30 minutes rolling in pot, then place 18 hours, at 110 ℃ dry 5 hours.Take after weight and be placed in again and roll pot, under rotation condition, in pot, spray into 35ml with atomizing type again and contain 15.3g basic cobaltous carbonate to rolling, 2.4g grass aqueous acid, after solution has sprayed, be rotated further 30 minutes rolling in pot, then place 18 hours, at 110 ℃, be dried 5 hours, make finished catalyst C.
Embodiment 4
100 g alumina supports are placed in and roll pot, under rotation condition, spray into 80ml with atomizing type and contain 2.5g molybdenum trioxide to rolling alumina support in pot, 13.7g ammonium metatungstate, the aqueous solution of 0.8g ethylene glycol, after solution has sprayed, is rotated further 30 minutes rolling in pot, then place 18 hours, at 110 ℃, be dried 5 hours.Take after weight and be placed in again and roll pot, under rotation condition, in pot, spray into 35ml with atomizing type again and contain 14.2g basic nickel carbonate to rolling, 3.7g lemon aqueous acid, after solution has sprayed, be rotated further 30 minutes rolling in pot, then place 18 hours, at 110 ℃, be dried 5 hours, make finished catalyst D.
Embodiment 5
On 200ml fixed bed small hydrogenation device, adopt respectively A, B, C, D catalyst, volume space velocity 2.0h in the time of hydrogen dividing potential drop 4.0MPa, liquid
-1, hydrogen to oil volume ratio is 300 Nm
3/ m
3, average reaction temperature is under 350 ℃ of conditions, his-and-hers watches 1 Raw hydrotreatment.
Table 1 feedstock property
| Feedstock oil | Atmosphere 3rd side cut straight-run diesel oil |
| Density (20 ℃), g/cm 3 | 0.8533 |
| Boiling range (ASTM-D86), ℃ | |
| IBP/10% | 217/277 |
| 30%/50% | 296/309 |
| 70%/90% | 327/356 |
| 95%/FBP | 369/375 |
| Sulfur content, μ g/g | 17750 |
| Nitrogen content, μ g/g | 140 |
Comparative example 1
100 g alumina supports are placed in and roll pot, under rotation condition, spray into 80ml with atomizing type and contain 22.9g molybdenum trioxide, 18.7g basic cobaltous carbonate, 0.9g ethylene glycol to rolling alumina support in pot, 4.7g lemon aqueous acid, after solution has sprayed, be rotated further 30 minutes rolling in pot, then place 18 hours, at 110 ℃, be dried 5 hours, make finished catalyst E.
Comparative example 2
100 g alumina supports are placed in and roll pot, under rotation condition, spray into 80ml with atomizing type and contain 22.9g molybdenum trioxide to rolling alumina support in pot, 18.7g basic cobaltous carbonate, 13.0g grass aqueous acid, after solution has sprayed, be rotated further 30 minutes rolling in pot, then place 18 hours, at 110 ℃, be dried 5 hours, make finished catalyst F.
Comparative example 3
100 g alumina supports are placed in and roll pot, under rotation condition, spray into 80ml with atomizing type and contain 22.9g molybdenum trioxide to rolling alumina support in pot, 18.7g basic cobaltous carbonate, the aqueous solution of 7.7g ethylene glycol, after solution has sprayed, be rotated further 30 minutes rolling in pot, then place 18 hours, at 110 ℃, be dried 5 hours, make finished catalyst G.
Comparative example 4
100 g alumina supports are placed in and roll pot, under rotation condition, spray into 80ml with atomizing type and contain 21.9g molybdenum trioxide, 10.1g basic cobaltous carbonate, 0.8g ethylene glycol to rolling alumina support in pot, 4.5g lemon aqueous acid, after solution has sprayed, be rotated further 30 minutes rolling in pot, then place 18 hours, at 110 ℃, be dried 5 hours, make finished catalyst H.
Comparative example 5
100 g alumina supports are placed in and roll pot, under rotation condition, spray into 80ml with atomizing type and contain 22.9g molybdenum trioxide to rolling alumina support in pot, 1.2g lemon aqueous acid, after solution has sprayed, be rotated further 30 minutes rolling in pot, then place 18 hours, at 110 ℃ dry 5 hours.Take after weight and be placed in again and roll pot, under rotation condition, in pot, spray into 35ml with atomizing type again and contain 15.3g basic cobaltous carbonate to rolling, 3.8g lemon aqueous acid, after solution has sprayed, be rotated further 30 minutes rolling in pot, then place 18 hours, at 110 ℃, be dried 5 hours, make finished catalyst I.
Comparative example 6
100 g alumina supports are placed in and roll pot, under rotation condition, spray into 80ml with atomizing type and contain 21.9g molybdenum trioxide to rolling alumina support in pot, the aqueous solution of 0.8g ethylene glycol, after solution has sprayed, be rotated further 30 minutes rolling in pot, then place 18 hours, at 110 ℃ dry 5 hours.Take after weight and be placed in again and roll pot, under rotation condition, in pot, spray into 35ml with atomizing type again and contain 8.3g basic cobaltous carbonate to rolling, 3.7g lemon aqueous acid, after solution has sprayed, be rotated further 30 minutes rolling in pot, then place 18 hours, at 110 ℃, be dried 5 hours, make finished catalyst J.
Comparative example 7
Evaluate catalysts E, F, G, H, I, J respectively, evaluation method is with embodiment 4.
Embodiment 6
The comparing result that this example turns round 600 hours for above each routine institute controlling catalyst physico-chemical property and above each example on small hydrogenation device is in table 2,3.
Table 2 catalyst main character
| Catalyst numbering | A | B | C | D |
| Catalyst property | ||||
| MoO 3，wt% | 17.0 | 16.0 | 17.0 | 2.0 |
| CoO，wt% | 8.0 | 9.0 | 8.0 | - |
| NiO，wt% | - | - | - | 6.0 |
| WO 3，wt% | - | - | - | 11.0 |
| C，wt% | 1.5 | 1.4 | 1.2 | 1.5 |
| From organic acid C/ VIII metal molar ratio | 0.16 | 0.13 | 0.23 | 0.21 |
| From the C/ vib metal mol ratio of Organic Alcohol | 0.05 | 0.06 | 0.14 | 0.10 |
| CoO /(CoO+MoO 3) weight ratio | 0.32 | 0.36 | 0.32 | |
| NiO/(NiO+MoO 3+WO 3) weight ratio | - | - | - | 0.32 |
| Preparation method | The present invention | The present invention | The present invention | The present invention |
| Pore volume, ml/g | 0.36 | 0.37 | 0.37 | 0.35 |
| Specific area, m 2/g | 244 | 245 | 247 | 238 |
| Bulk density, g/ml | 0.90 | 0.90 | 0.89 | 0.86 |
| Intensity, N/ unit | 205 | 207 | 212 | 208 |
Continued 2
| Catalyst numbering | E | F | G | H | I | J |
| Catalyst property | ||||||
| MoO 3，wt% | 17.0 | 17.0 | 17.0 | 17.0 | 17.0 | 17.0 |
| CoO，wt% | 8.0 | 8.0 | 8.0 | 4.5 | 8.0 | 4.5 |
| NiO，wt% | - | - | - | - | - | - |
| WO 3，wt% | - | - | - | - | - | - |
| C，wt% | 1.5 | 2.6 | 2.6 | 1.5 | 1.5 | 1.5 |
| From organic acid C/ VIII metal molar ratio | 0.16 | 1.02 | - | 0.21 | 0.16 | 0.21 |
| From the C/ vib metal mol ratio of Organic Alcohol | 0.05 | - | 0.46 | 0.05 | - | 0.05 |
| From organic acid C/ vib metal mol ratio | - | - | - | - | 0.05 | - |
| CoO /(CoO+MoO 3) weight ratio | 0.32 | 0.32 | 0.32 | 0.21 | 0.32 | 0.21 |
| NiO/(NiO+MoO 3+WO 3) weight ratio | ||||||
| Preparation method | Total immersion method | Total immersion method | Total immersion method | Total immersion method | Sub-dip method | Sub-dip method |
| Pore volume, ml/g | 0.34 | 0.35 | 0.35 | 0.38 | 0.35 | 0.39 |
| Specific area, m 2/g | 208 | 201 | 203 | 210 | 217 | 212 |
| Bulk density, g/ml | 0.90 | 0.91 | 0.91 | 0.87 | 0.89 | 0.88 |
| Intensity, N/ unit | 175 | 184 | 186 | 189 | 192 | 195 |
The activity level of table 3 catalyst
| Catalyst numbering | A | B | C | D | E | F | G | H | I | J |
| Process conditions | ||||||||||
| Hydrogen dividing potential drop, MPa | 4.0 | 4.0 | 4.0 | 4.0 | 4.0 | 4.0 | 4.0 | 4.0 | 4.0 | 4.0 |
| Volume space velocity, h -1 | 2.0 | 2.0 | 2.0 | 2.0 | 2.0 | 2.0 | 2.0 | 2.0 | 2.0 | 2.0 |
| Reaction temperature, ℃ | 350 | 350 | 350 | 350 | 350 | 350 | 350 | 350 | 350 | 350 |
| Generate oil nature | ||||||||||
| Sulphur, μ g/g | 288 | 286 | 292 | 307 | 328 | 390 | 386 | 366 | 322 | 329 |
| Nitrogen, μ g/g | 9.8 | 9.1 | 9.4 | 8.2 | 14.6 | 25.6 | 24.9 | 20.1 | 13.2 | 14.9 |
Table 3 result shows, catalyst of the present invention has better hydrotreatment activity, has better ultra-deep desulfurization, nitrogen removal performance compared with comparative catalyst.
Claims (10)
1. the preparation method of a catalyst for hydrogenation of fraction oil, described catalyst is take aluminium oxide as carrier, take at least one group vib metal and at least one group VIII metal as hydrogenation active metals, in catalyst, contain organic compound, organic compound come from organic acid and be selected from Organic Alcohol and organic sugar at least one, this catalyst is to adopt infusion process load regulation group vib metal on alumina support, group VIII metal and organic compound, the addition of organic compound accounts for the 1.0wt% ~ 1.8wt% of hydrotreating catalyst weight in C, process comprises:
(1) prepare respectively dipping solution I and dipping solution II, wherein dipping solution I be by containing group vib metal with to be selected from least one and water in Organic Alcohol and organic sugar formulated, dipping solution II is by formulated containing group VIII metallic compound and organic acid, water, wherein organic acid addition take C with the mol ratio of group VIII metal as 0.01 ~ 0.70, be selected from least one in Organic Alcohol and organic sugar take C with the mol ratio of group vib metal as 0.01 ~ 0.40;
(2) first use dipping solution I oxide impregnation alumina supporter, after dry at the temperature below 200 ℃, then with dipping solution II dipping, dry at the temperature below 200 ℃, obtain hydrotreating catalyst.
2. in accordance with the method for claim 1, it is characterized in that in described hydrotreating catalyst, take the weight of catalyst as benchmark, hydrogenation active metals is take the weight content of oxide as 14% ~ 50%.
3. in accordance with the method for claim 1, it is characterized in that in described hydrotreating catalyst, take the weight of catalyst as benchmark, hydrogenation active metals is take the weight content of oxide as 15% ~ 40%.
4. according to the method described in claim 1,2 or 3, it is characterized in that in described hydrotreating catalyst, group VIII metal/(group vib metal+group VIII metal) is take the weight ratio of oxide as 0.30 ~ 0.55.
5. in accordance with the method for claim 1, it is characterized in that in described hydrotreating catalyst, group vib metal is Mo and/or W, group VIII metal is Ni and/or Co.
6. in accordance with the method for claim 1, it is characterized in that the addition of described organic compound accounts for 1.2 wt% ~ 1.6 wt % of hydrotreating catalyst weight in C.
7. in accordance with the method for claim 1, it is characterized in that it is at least one in 2 ~ 10 binary acid that described organic acid is selected from carbon number; It is one or more in 3 ~ 10 fatty alcohol and dihydroxylic alcohols that described Organic Alcohol is selected from carbon number; It is at least one in 3 ~ 10 monose, disaccharides and polysaccharide that described organic sugar is selected from carbon number.
8. in accordance with the method for claim 1, it is characterized in that described organic acid is one or more in citric acid, citric anhydride, isocitric acid, malic acid, tartaric acid, oxalic acid, butanedioic acid, glutaric acid, adipic acid, benzoic acid, phthalandione, isophathalic acid, salicylic acid, malonic acid; Described Organic Alcohol is one or more in fatty alcohol, ethylene glycol, propyleneglycoles, glycerine, three methylol ethane, three methylol propane, divinyl ethylene glycol, two propyleneglycoles, trimethylene ethylene glycol, trietbhlene glycol, tributylene glycol, tetrem allyl diglycol, tetrapropylene ethylene glycol, polyethylene glycol, divinyl Propylene Glycol, divinyl ethohexadiol, divinyl propyl glycol, divinyl butyl glycol; It is at least one in 3 ~ 10 monose, disaccharides and polysaccharide that described organic sugar is selected from carbon number.
9. in accordance with the method for claim 1, it is characterized in that containing phosphorus in described hydrotreating catalyst, the weight content in catalyst is 0.01% ~ 2.5%.
10. in accordance with the method for claim 1, it is characterized in that: while adopting dipping solution I or dipping solution II to flood, adopt the saturated method that sprays, adopt one or many dipping, all dry through 200 ℃ of following temperature after each dipping.
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